CN104193830A - Method for producing cellulose ether by taking dimethyl carbonate substituted chloromethane as etherifying agent - Google Patents
Method for producing cellulose ether by taking dimethyl carbonate substituted chloromethane as etherifying agent Download PDFInfo
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- CN104193830A CN104193830A CN201410405326.2A CN201410405326A CN104193830A CN 104193830 A CN104193830 A CN 104193830A CN 201410405326 A CN201410405326 A CN 201410405326A CN 104193830 A CN104193830 A CN 104193830A
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- Prior art keywords
- cellulose ether
- methylcarbonate
- dimethyl carbonate
- etherifying agent
- chloromethane
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- NEHMKBQYUWJMIP-UHFFFAOYSA-N anhydrous methyl chloride Natural products ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 28
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 21
- 229920003086 cellulose ether Polymers 0.000 title claims abstract description 20
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical group COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 title abstract description 13
- NEHMKBQYUWJMIP-OUBTZVSYSA-N chloromethane Chemical class Cl[13CH3] NEHMKBQYUWJMIP-OUBTZVSYSA-N 0.000 title abstract 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 36
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 35
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 238000010792 warming Methods 0.000 claims abstract description 14
- 229920000742 Cotton Polymers 0.000 claims abstract description 12
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 claims abstract description 12
- CXHHBNMLPJOKQD-UHFFFAOYSA-M methyl carbonate Chemical compound COC([O-])=O CXHHBNMLPJOKQD-UHFFFAOYSA-M 0.000 claims description 33
- 238000000034 method Methods 0.000 claims description 22
- 229940050176 methyl chloride Drugs 0.000 claims description 22
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 18
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 claims description 11
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 claims description 11
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 claims description 10
- UFVKGYZPFZQRLF-UHFFFAOYSA-N hydroxypropyl methyl cellulose Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(O)C(CO)O3)O)C(CO)O2)O)C(CO)O1 UFVKGYZPFZQRLF-UHFFFAOYSA-N 0.000 claims description 10
- YLGXILFCIXHCMC-JHGZEJCSSA-N methyl cellulose Chemical compound COC1C(OC)C(OC)C(COC)O[C@H]1O[C@H]1C(OC)C(OC)C(OC)OC1COC YLGXILFCIXHCMC-JHGZEJCSSA-N 0.000 claims description 10
- 239000000047 product Substances 0.000 abstract description 16
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 abstract description 14
- 239000002994 raw material Substances 0.000 abstract description 7
- 239000002699 waste material Substances 0.000 abstract description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 3
- 239000006227 byproduct Substances 0.000 abstract description 2
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 238000001035 drying Methods 0.000 abstract 2
- 238000005406 washing Methods 0.000 abstract 2
- 239000001569 carbon dioxide Substances 0.000 abstract 1
- 229910002092 carbon dioxide Inorganic materials 0.000 abstract 1
- 238000001816 cooling Methods 0.000 abstract 1
- 239000011259 mixed solution Substances 0.000 abstract 1
- 241000219146 Gossypium Species 0.000 description 10
- 125000005911 methyl carbonate group Chemical class 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 229920002678 cellulose Polymers 0.000 description 4
- 239000001913 cellulose Substances 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 239000004570 mortar (masonry) Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 231100000252 nontoxic Toxicity 0.000 description 3
- 230000003000 nontoxic effect Effects 0.000 description 3
- NIQCNGHVCWTJSM-UHFFFAOYSA-N Dimethyl phthalate Chemical compound COC(=O)C1=CC=CC=C1C(=O)OC NIQCNGHVCWTJSM-UHFFFAOYSA-N 0.000 description 2
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- NEHMKBQYUWJMIP-NJFSPNSNSA-N chloro(114C)methane Chemical compound [14CH3]Cl NEHMKBQYUWJMIP-NJFSPNSNSA-N 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- -1 hydroxypropyl Chemical group 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 description 2
- 239000002574 poison Substances 0.000 description 2
- 239000003440 toxic substance Substances 0.000 description 2
- FRXSZNDVFUDTIR-UHFFFAOYSA-N 6-methoxy-1,2,3,4-tetrahydroquinoline Chemical compound N1CCCC2=CC(OC)=CC=C21 FRXSZNDVFUDTIR-UHFFFAOYSA-N 0.000 description 1
- JVFDADFMKQKAHW-UHFFFAOYSA-N C.[N] Chemical compound C.[N] JVFDADFMKQKAHW-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 235000011089 carbon dioxide Nutrition 0.000 description 1
- 230000006315 carbonylation Effects 0.000 description 1
- 238000005810 carbonylation reaction Methods 0.000 description 1
- 239000003183 carcinogenic agent Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- FBSAITBEAPNWJG-UHFFFAOYSA-N dimethyl phthalate Natural products CC(=O)OC1=CC=CC=C1OC(C)=O FBSAITBEAPNWJG-UHFFFAOYSA-N 0.000 description 1
- 229960001826 dimethylphthalate Drugs 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 238000006266 etherification reaction Methods 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- OJURWUUOVGOHJZ-UHFFFAOYSA-N methyl 2-[(2-acetyloxyphenyl)methyl-[2-[(2-acetyloxyphenyl)methyl-(2-methoxy-2-oxoethyl)amino]ethyl]amino]acetate Chemical compound C=1C=CC=C(OC(C)=O)C=1CN(CC(=O)OC)CCN(CC(=O)OC)CC1=CC=CC=C1OC(C)=O OJURWUUOVGOHJZ-UHFFFAOYSA-N 0.000 description 1
- 230000001035 methylating effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 231100000004 severe toxicity Toxicity 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Landscapes
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention relates to a method for producing cellulose ether by taking dimethyl carbonate substituted chloromethane as an etherifying agent. The method for producing the cellulose ether by taking the dimethyl carbonate substituted chloromethane as the etherifying agent comprises the following steps: firstly, mixing methylbenzene, isopropanol and water; (2) adding sodium hydroxide into a mixed solution, and dissolving; (3) adding purified cotton, alkalifying, and then cooling; (4) adding dimethyl carbonate, warming for reaction, centrifuging, washing products with hot water, and then centrifuging and drying; or adding dimethyl carbonate and epoxy propane, warming for reaction, centrifuging and washing products with hot water, and then centrifuging and drying. The method for producing the cellulose ether by taking the dimethyl carbonate substituted chloromethane as the etherifying agent has the advantages that dimethyl carbonate is taken as a raw material, and the reaction activity of the dimethyl carbonate is far higher than that of chloromethane, so that the reaction efficiency is improved, and waste of the raw material is greatly reduced; a methyl alcohol byproduct produced in a reaction process can be directly generated into dimethyl carbonate with carbon dioxide under a supercritical condition, so that environmental pollution is effectively controlled.
Description
Technical field
The present invention relates to a kind of methylcarbonate and replace methyl chloride as the method for etherifying agent production of cellulose ether, belong to the technical field of the production technology of ether of cellulose.
Background technology
China's mortar output occupies first place in the world, and even world wide production is partly near.Its technology is just progressively close to complex function type mortar, and a large amount of new additive agents are used in the production of concrete and mortar thereupon, to product, have brought various effect.Ether of cellulose is a kind of as these additives, has been widely used among all kinds of concrete and mortar production technique.
Yet producing HPMC at present, in the technological process of MC and MHEC, mostly adopt methyl chloride as methylating reagent, itself is for needing pressurized liquefied high-risk, the inflammable obnoxious flavour with steel cylinder accumulating, more and more restricted, and methyl chloride reactive behavior is low, conventionally in the reaction of Mierocrystalline cellulose etherificate, only have less than 50% that etherification reaction occurs, most residual nitrogen methane is but converted into methyl alcohol in alkaline environment, the almost unavoidable profligacy of raw material and the severe contamination of environment of having caused.The degraded that high salinity (sodium-chlor) also makes COD is difficulty very, there is no what thalline can be under the salinity of 4% left and right effective degradation of organic substances.This is also the problem that nearly all ether of cellulose manufacturer faces now.
Methylcarbonate (being called for short DMC) is the green chemical industry product that the eighties in last century Europe and the U.S. develop respectively novel process suitability for industrialized production, recently with domestic by extensive concern.DMC in 1992, by the registration of European non-toxic chemicals (Non toxic substance), is regarded as Green Chemistry reagent in the U.S., belongs to nontoxic or micro-chemical product that poisons.Be expected to substitute that many severe toxicity or carcinogenic substance carry out a carbonylation, methylate, the reaction such as esterification and transesterify generates multiple important Chemicals.
The character of carbon element dimethyl ester: molecular formula (CH
30)
2c=0CAS; Number 616-38-6; Molecular weight 90.08; Relative density 1.070; Specific refractory power 1.3697; 4 ℃ of fusing points; 90.1 ℃ of boiling points.Under normal temperature, be colourless liquid, have combustibility, be slightly soluble in water but there is the ability that forms azeotrope with water, can with nearly all immiscible organic solvent such as alcohol, ether, ketone.To metal non-corrosiveness, the accumulating of available metal bucket splendid attire.Micro-poison (LD50=6400 ~ 12900mg/kg, methyl alcohol is LD50=3000mg/kg).
Therefore, methylcarbonate replacement methyl chloride is that the technical barrier of capturing is badly in need of in this area as etherifying agent production of cellulose ether.
Summary of the invention
For the above-mentioned technical problem of prior art, the object of this invention is to provide a kind of methylcarbonate and replace methyl chloride as the method for etherifying agent production of cellulose ether, to reach the more object of optimizing product production technique.
For achieving the above object, the present invention is achieved by the following technical solutions:
Methylcarbonate replaces methyl chloride as a method for etherifying agent production of cellulose ether, comprises the following steps:
(1) toluene, isopropyl alcohol and water are mixed than 75-85:15-25:0.5-2 by mass parts;
(2) 5-8 part sodium hydroxide is added in the mixing solutions of step (1), then 60-80 ℃ of dissolving;
(3) in the solution of step (2), add 8-10 part purified cotton, the 40-60 minute that then alkalizes at 50-80 ℃, then be cooled to 30-50 ℃;
(4) in the solution of step (3), add 15-20 part methylcarbonate, react 8-10 hour after being warming up to 80-100 ℃, centrifugal rear 90-95 ℃ hot wash product, and then centrifugal and dry;
Or in the solution of step (3), add 15-20 part methylcarbonate and 2-4 part propylene oxide, and react 8-10 hour after being warming up to 80-100 ℃, centrifugal rear 90-95 ℃ hot wash product, and then centrifugal and dry.
While adding methylcarbonate in described step (4), described reaction equation is as follows:
。
While adding methylcarbonate and propylene oxide in described step (4), described reaction equation is as follows:
。
As preferably, while adding methylcarbonate in described step (4), make methyl cellulose ether.
As preferably, while adding methylcarbonate and propylene oxide in described step (4), make hydroxypropyl methyl cellulose ether.
Beneficial effect of the present invention is as follows:
1, the present invention be take methylcarbonate as raw material, thereby dimethyl carbonate activity improves reaction efficiency higher than methyl chloride far away, reduces significantly the waste of raw material; The by-product carbinol producing in its reaction process can be under super critical condition and the direct Formed dimethyl phthalate of carbonic acid gas, and environmental pollution is effectively controlled.
2, methylcarbonate normal temperature is liquid, and accumulating is all better than methyl chloride.
3, methylcarbonate toxicity is low, non-stimulated to human body skin, is easy to biological degradation.
4, liquid state can improve operability, production efficiency and the technique that simplifies the operation to production process, because equipment does not need high pressure resistantly, thereby can reduce to a certain extent, the technical requirements of equipment is further cut operating costs.
5, the most important thing is, because reaction itself does not produce sodium-chlor, for the wastewater treatment of high COD brings hope.
Accompanying drawing explanation
Fig. 1 is the infrared spectrogram of the hydroxypropyl methyl cellulose ether produced of the hydroxypropyl methyl cellulose ether that makes of the present invention and traditional technology;
Fig. 2 is the infrared spectrogram of the methyl cellulose ether produced of the methyl cellulose ether that makes of the present invention and traditional technology;
Fig. 3 is the hydroxypropyl of hydroxypropyl methyl cellulose ether and the gas chromatogram of methoxy content mensuration that the present invention makes;
Fig. 4 is the interpretation of result figure of Fig. 3;
Fig. 5 is the hydroxypropyl of methyl cellulose ether and the gas chromatogram of methoxy content mensuration that the present invention makes;
Fig. 6 is the interpretation of result figure of Fig. 5.
Embodiment
Below in conjunction with specific embodiment, the present invention is further illustrated, but protection scope of the present invention is not limited to this.
Raw material toluene, Virahol, water, sodium hydroxide, purified cotton, methylcarbonate and propylene oxide in the present invention all can adopt commercially available prod, also can make by means commonly known in the art.
embodiment 1
Methylcarbonate of the present invention replaces methyl chloride as the method for etherifying agent production of cellulose ether, comprises the following steps:
(1) toluene, isopropyl alcohol and water are mixed than 85:25:2 by mass parts;
(2) 8 parts of sodium hydroxide are added in the mixing solutions of step (1), then 80 ℃ of dissolvings;
(3) in the solution of step (2), add 10 parts of purified cottons, then at 80 ℃, alkalize 60 minutes, then be cooled to 50 ℃;
(4) in the solution of step (3), add 20 parts of methylcarbonates, react 10 hours after being warming up to 100 ℃, centrifugal rear 95 ℃ of hot wash products, and then centrifugal and dry, make methyl cellulose ether.
embodiment 2
Methylcarbonate of the present invention replaces methyl chloride as the method for etherifying agent production of cellulose ether, comprises the following steps:
(1) toluene, isopropyl alcohol and water are mixed than 75:15:0.5 by mass parts;
(2) 5 parts of sodium hydroxide are added in the mixing solutions of step (1), then 60 ℃ of dissolvings;
(3) in the solution of step (2), add 8 parts of purified cottons, then at 50 ℃, alkalize 40 minutes, then be cooled to 30 ℃;
(4) in the solution of step (3), add 15 parts of methylcarbonates, react 80 hours after being warming up to 80 ℃, centrifugal rear 905 ℃ of hot wash products, and then centrifugal and dry; Make methyl cellulose ether.
embodiment 3
Methylcarbonate of the present invention replaces methyl chloride as the method for etherifying agent production of cellulose ether, comprises the following steps:
(1) toluene, isopropyl alcohol and water are mixed than 80:20:1.25 by mass parts;
(2) 6.5 parts of sodium hydroxide are added in the mixing solutions of step (1), then 70 ℃ of dissolvings;
(3) in the solution of step (2), add 9 parts of purified cottons, then at 65 ℃, alkalize 50 minutes, then be cooled to 40 ℃;
(4) in the solution of step (3), add 17.5 parts of methylcarbonates, react 9 hours after being warming up to 90 ℃, centrifugal rear 92.5 ℃ of hot wash products, and then centrifugal and dry, make methyl cellulose ether.
embodiment 4
Methylcarbonate of the present invention replaces methyl chloride as the method for etherifying agent production of cellulose ether, comprises the following steps:
(1) toluene, isopropyl alcohol and water are mixed than 85:25:2 by mass parts;
(2) 8 parts of sodium hydroxide are added in the mixing solutions of step (1), then 80 ℃ of dissolvings;
(3) in the solution of step (2), add 10 parts of purified cottons, then at 80 ℃, alkalize 60 minutes, then be cooled to 50 ℃;
(4) in the solution of step (3), add 20 parts of methylcarbonates and 4 parts of propylene oxide, react 10 hours after being warming up to 100 ℃, centrifugal rear 95 ℃ of hot wash products, and then centrifugal and dry, make hydroxypropyl methyl cellulose ether.
embodiment 5
Methylcarbonate of the present invention replaces methyl chloride as the method for etherifying agent production of cellulose ether, comprises the following steps:
(1) toluene, isopropyl alcohol and water are mixed than 80:20:1.25 by mass parts;
(2) 6.5 parts of sodium hydroxide are added in the mixing solutions of step (1), then 70 ℃ of dissolvings;
(3) in the solution of step (2), add 9 parts of purified cottons, then at 65 ℃, alkalize 50 minutes, then be cooled to 40 ℃;
(4) in the solution of step (3), add 17.5 parts of methylcarbonates and 3 parts of propylene oxide, react 9 hours after being warming up to 90 ℃, centrifugal rear 92.5 ℃ of hot wash products, and then centrifugal and dry, make hydroxypropyl methyl cellulose ether.
embodiment 6
Methylcarbonate of the present invention replaces methyl chloride as the method for etherifying agent production of cellulose ether, comprises the following steps:
(1) toluene, isopropyl alcohol and water are mixed than 75:15:0.5 by mass parts;
(2) 5 parts of sodium hydroxide are added in the mixing solutions of step (1), then 60 ℃ of dissolvings;
(3) in the solution of step (2), add 8 parts of purified cottons, then at 50 ℃, alkalize 40 minutes, then be cooled to 30 ℃;
(4) in the solution of step (3), add 15 parts of methylcarbonates and 2 parts of propylene oxide, react 8 hours after being warming up to 80 ℃, centrifugal rear 90 ℃ of hot wash products, and then centrifugal and dry, make hydroxypropyl methyl cellulose ether.
comparative example 1
The method that this comparative example 1 is produced hydroxypropyl methyl cellulose ether for traditional technology, comprises the following steps:
(1) toluene, isopropyl alcohol and water are mixed than 86:10:4 by mass parts;
(2) 2.5 parts of sodium hydroxide are added in 40 parts of the mixing solutionss of step (1), then 70 ℃ of dissolvings;
(3) in the solution of step (2), add 3.8 parts of purified cottons, then at 65 ℃, alkalize 50 minutes, then be cooled to 20 ℃;
(4) in the solution of step (3), add 3.5 methyl chloride and 1 part of propylene oxide, react 5 hours after being warming up to gradually 90 ℃, centrifugal rear 90 ℃ of hot wash products, and then centrifugal and dry, make hydroxypropyl methyl cellulose ether.
comparative example 2
The method that this comparative example 2 is produced methyl cellulose ether for traditional technology, comprises the following steps:
(1) toluene, isopropyl alcohol and water are mixed than 86:10:4 by mass parts;
(2) 2.5 parts of sodium hydroxide are added in 40 parts of the mixing solutionss of step (1), then 70 ℃ of dissolvings;
(3) in the solution of step (2), add 3.8 parts of purified cottons, then at 65 ℃, alkalize 50 minutes, then be cooled to 20 ℃;
(4) in the solution of step (3), add 3.5 methyl chloride, react 3 hours after being warming up to 65 ℃, centrifugal rear 90 ℃ of hot wash products, and then centrifugal and dry, make methyl cellulose ether.
In comparative example 1 and 2, in methylated reaction process, the practical efficiency of methyl chloride is only 40% left and right, not only causes the waste of raw material, and brings high salinity and methanol waste liquid.Reactive behavior in embodiment 1-6 is far above methyl chloride, and practical efficiency is more than 80%.
Above-described embodiment is only for the inventive concept of the present invention of explaining, but not restriction to rights protection of the present invention, allly utilizes this design to carry out the change of unsubstantiality to the present invention, all should fall into protection scope of the present invention.
Claims (5)
1. methylcarbonate replaces methyl chloride as the method for etherifying agent production of cellulose ether, it is characterized in that comprising the following steps:
(1) toluene, isopropyl alcohol and water are mixed than 75-85:15-25:0.5-2 by mass parts;
(2) 5-8 part sodium hydroxide is added in the mixing solutions of step (1), then 60-80 ℃ of dissolving;
(3) in the solution of step (2), add 8-10 part purified cotton, the 40-60 minute that then alkalizes at 50-80 ℃, then be cooled to 30-50 ℃;
(4) in the solution of step (3), add 15-20 part methylcarbonate, react 8-10 hour after being warming up to 80-100 ℃, centrifugal rear 90-95 ℃ hot wash product, and then centrifugal and dry;
Or in the solution of step (3), add 15-20 part methylcarbonate and 2-4 part propylene oxide, and react 8-10 hour after being warming up to 80-100 ℃, centrifugal rear 90-95 ℃ hot wash product, and then centrifugal and dry.
2. methylcarbonate replaces methyl chloride as the method for etherifying agent production of cellulose ether as claimed in claim 1, and while it is characterized in that adding methylcarbonate in step (4), described reaction equation is as follows:
。
3. methylcarbonate replaces methyl chloride as the method for etherifying agent production of cellulose ether as claimed in claim 1 or 2, it is characterized in that: while adding methylcarbonate in described step (4), make methyl cellulose ether.
4. methylcarbonate replaces methyl chloride as the method for etherifying agent production of cellulose ether as claimed in claim 1, and while it is characterized in that adding methylcarbonate and propylene oxide in step (4), described reaction equation is as follows:
。
5. as described in claim 1 or 4, methylcarbonate replaces methyl chloride as the method for etherifying agent production of cellulose ether, it is characterized in that: while adding methylcarbonate and propylene oxide in described step (4), make hydroxypropyl methyl cellulose ether.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104558204A (en) * | 2015-01-20 | 2015-04-29 | 西安理工大学 | Green quick high-efficiency methylation method of cellulose |
| CN104558202A (en) * | 2015-01-20 | 2015-04-29 | 西安理工大学 | Green preparation method of methyl cellulose |
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| CN102816247A (en) * | 2012-08-20 | 2012-12-12 | 新疆光大山河化工科技有限公司 | Preparation method of ultra-low-viscosity hydroxypropyl methyl cellulose |
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2014
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