CN102690356A - Preparation method of hydroxyl-ethyl methyl cellulose - Google Patents
Preparation method of hydroxyl-ethyl methyl cellulose Download PDFInfo
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- CN102690356A CN102690356A CN2012101451860A CN201210145186A CN102690356A CN 102690356 A CN102690356 A CN 102690356A CN 2012101451860 A CN2012101451860 A CN 2012101451860A CN 201210145186 A CN201210145186 A CN 201210145186A CN 102690356 A CN102690356 A CN 102690356A
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Abstract
The invention discloses a preparation method of hydroxyl-ethyl methyl cellulose; according to the method, refined cotton is used as the raw material, and ethylene oxide is used as the etherifying agent so as to prepare hydroxyl-ethyl methyl cellulose; compared with the existing cellulose ether technology, the hydroxyl-ethyl methyl cellulose prepared by the method has advantages that as the ethylene oxide is used as the etherifying agent to prepare the hydroxyl-ethyl methyl cellulose, the anti-mildew ability is high due to the hydroxyethyl group, and hydroxyl-ethyl methyl cellulose prepared by the method is high in the viscosity stability and the anti-mildew ability when being stored for a long time and can replace other cellulose ethers.
Description
Technical field
The present invention relates to a kind of preparation method of hydroxyethylmethyl-cellulose.
Background technology
Hydroxyethylmethyl-cellulose (HEMC) main characteristic has:
Water-soluble and part organic solvent, HEMC can be dissolved in cold water, and its maximum concentration only is decided by viscosity, and solubleness changes with viscosity, and viscosity is lower, and solubleness is bigger.
Salt resistance: the HEMC product is the non-ionic type ether of cellulose, and is not polyelectrolyte, and is therefore when metal-salt or organic electrolyte exist, more stable in the aqueous solution, but excessive interpolation ionogen can cause gel and deposition.
Surfactivity:, can be used as colloid protective agent, emulsifying agent and dispersion agent because the aqueous solution has surface active function.
Hot gel: the HEMC product aqueous solution becomes opaque, gel when being heated to certain temperature; Form deposition, but when cooling off continuously, then return to original solution state again; And this gel takes place and temperature of precipitation depends primarily on their lubricants; Suspension aid, protective colloid, emulsifying agent etc.
Metabolism inertia and low smell and fragrance: because therefore HEMC can not used in food and medicine by metabolism and low smell and fragrance widely.
Mould resistance: HEMC has reasonable anti-mildew ability, and good viscosity stability is arranged when standing storage.
PH stability: HEMC product viscosity in aqueous solution is the influence of acid and alkali or alkali almost, and pH value is more stable in the scope of 3.0-11.0.
Hydroxyethylmethyl-cellulose is that a kind of nothing is smelt, tasteless, nontoxic white powder, can be dissolved in cold water, forms transparent viscous solution.Have characteristics such as thickening, bonding, dispersion, emulsification, film forming, suspension, absorption, gelling, surfactivity, maintenance moisture and protective colloid.Because the aqueous solution has surface active function, can be used as colloid protective agent, emulsifying agent and dispersion agent.The hydroxyethylmethyl-cellulose aqueous solution has good hydrophilicity, is a kind of high-performance water-retaining agent.
Hydroxyethylmethyl-cellulose so have good anti-mildew ability, has good viscosity stability and anti-mildew sex change because of containing hydroxyethyl groups during standing storage.
Hydroxyethylmethyl-cellulose (HEMC) is in methylcellulose gum (MC), to introduce oxyethane substituting group (MS 0.3～0.4) to make, and its salt tolerance is better than unmodified polymer, and the gelling temp of hydroxyethylmethyl-cellulose is also high than MC.
Summary of the invention
The technical issues that need to address of the present invention just are to provide a kind of preparation method of hydroxyethylmethyl-cellulose; With existing ether of cellulose compared with techniques; The present invention produces hydroxyethylmethyl-cellulose, because of containing hydroxyethyl groups owing to adopt oxyethane as etherifying agent; Have good anti-mildew ability, good viscosity stability and anti-mildew sex change are arranged during standing storage.Alternative other ether of cellulose uses.
For addressing the above problem, the present invention adopts following technical scheme:
The invention provides a kind of preparation method of hydroxyethylmethyl-cellulose, said method be with purified cotton as raw material, adopt oxyethane as etherifying agent, produce hydroxyethylmethyl-cellulose.
Among the present invention, the parts by weight of raw materials of preparation hydroxyethylmethyl-cellulose is provided as: toluene and isopropanol mixture are made solvent for 700～800 parts, 30～40 parts in water; 70～80 parts in sodium hydroxide, 80～85 parts of purified cottons, 20～28 parts in oxyethane; 80～90 parts of methyl chloride, 16～19 parts in Glacial acetic acid min. 99.5;
Concrete steps are:
The first step in reaction kettle, adds toluene and isopropanol mixture, water and sodium hydroxide, is warming up to 60～80 ℃, is incubated 20～40 minutes;
Second step, alkalization: above-mentioned material is cooled to 30～50 ℃, adds purified cotton; Carry out toluene and isopropanol mixture solvent spray; Be evacuated to-0.006Mpa, inflated with nitrogen carries out 3 displacements, replaces the laggard row alkalization that finishes; The alkalization condition is: alkalization time is 2 hours, and alkalization temperature is 30 ℃-50 ℃;
In the 3rd step, etherificate: alkalization finishes, and reaction kettle is evacuated to 0.05～0.07MPa, adds oxyethane and methyl chloride, keeps 30～50 minutes; The etherificate fs: 40～60 ℃, 1.0～2.0 hours, pressure-controlling was between 0.15-0.3Mpa; The etherificate subordinate phase: 60～90 ℃, 2.0～2.5 hours, pressure-controlling was between 0.4-0.8Mpa;
In the 4th step, neutralization: add the Glacial acetic acid min. 99.5 that measures in advance at the precipitation still, be pressed into the intact material of etherificate and neutralize, heat up 75～80 ℃ and carry out precipitation, temperature rises to 102 ℃, is that precipitation finishes when detecting pH value for 6-8; Fill it up with 90 ℃～100 ℃ the tap water of crossing through the reverse osmosis apparatus processes at the precipitation still;
In the 5th step, centrifuge washing: the material in the 4th step is carried out spinning through horizontal spiral centrifuge, and separation of material is transferred to the washing still of filling it up with hot water in advance, carries out the washing of material;
In the 6th step, whiz: the material after the washing is conveyed into drying machine through horizontal spiral centrifuge, at 150～170 ℃ material is carried out drying, and the exsiccant material is pulverized the back packing.Compare with existing ether of cellulose production technology, the present invention produces hydroxyethylmethyl-cellulose owing to adopt oxyethane as etherifying agent, because of containing hydroxyethyl groups, has good anti-mildew ability, and good viscosity stability and anti-mildew sex change are arranged during standing storage.Alternative other ether of cellulose uses.
Embodiment
Embodiment 1
The parts by weight of raw materials that the present invention prepares hydroxyethylmethyl-cellulose is provided as: toluene and isopropanol mixture are made solvent for 700 parts, 40 parts in water, 70 parts in sodium hydroxide, 85 parts of purified cottons, 20 parts in oxyethane, 90 parts, 16 parts in Glacial acetic acid min. 99.5;
Concrete steps are:
The first step in reaction kettle, adds toluene and isopropanol mixture, water and sodium hydroxide, is warming up to 60 ℃, is incubated 40 minutes;
Second step, alkalization: above-mentioned material is cooled to 30 ℃, adds purified cotton; Carry out toluene and isopropanol mixture solvent spray, be evacuated to-0.006Mpa, inflated with nitrogen carries out 3 displacements; Replace the laggard row alkalization that finishes, the alkalization condition is: alkalization time is 2 hours, and alkalization temperature is 50 ℃;
In the 3rd step, etherificate: alkalization finishes, and reaction kettle is evacuated to 0.07MPa, adds oxyethane and methyl chloride, keeps 30 minutes; The etherificate fs: 40 ℃, 2.0 hours, pressure-controlling was at 0.15Mpa; The etherificate subordinate phase: 90 ℃, 2.0 hours, pressure-controlling was at 0.4Mpa;
In the 4th step, neutralization: add the Glacial acetic acid min. 99.5 that measures in advance at the precipitation still, be pressed into the intact material of etherificate and neutralize, heats up 75 ℃ and carry out precipitation, temperature rises to 102 ℃, the detection pH value be 6 o'clock be that precipitation finishes; Fill it up with 90 ℃ the tap water of crossing through the reverse osmosis apparatus processes at the precipitation still;
In the 5th step, centrifuge washing: the material in the 4th step is carried out spinning through horizontal spiral centrifuge, and separation of material is transferred to the washing still of filling it up with hot water in advance, carries out the washing of material;
In the 6th step, whiz: the material after the washing is conveyed into drying machine through horizontal spiral centrifuge, at 150 ℃ material is carried out drying, and the exsiccant material is pulverized the back packing.
Embodiment 2
The parts by weight of raw materials that the present invention prepares hydroxyethylmethyl-cellulose is provided as: toluene and isopropanol mixture are made solvent for 800 parts, 30 parts in water, 80 parts in sodium hydroxide, 80 parts of purified cottons, 28 parts in oxyethane, 80 parts of methyl chloride, 19 parts in Glacial acetic acid min. 99.5;
Concrete steps are:
The first step in reaction kettle, adds toluene and isopropanol mixture, water and sodium hydroxide, is warming up to 80 ℃, is incubated 20 minutes;
Second step, alkalization: above-mentioned material is cooled to 50 ℃, adds purified cotton; Carry out toluene and isopropanol mixture solvent spray, be evacuated to-0.006Mpa, inflated with nitrogen carries out 3 displacements; Replace the laggard row alkalization that finishes, the alkalization condition is: alkalization time is 2 hours, and alkalization temperature is 30 ℃;
In the 3rd step, etherificate: alkalization finishes, and reaction kettle is evacuated to 0.05MPa, adds oxyethane and methyl chloride, keeps 50 minutes; The etherificate fs: 60 ℃, 1.0 hours, pressure-controlling was between 0.3Mpa; The etherificate subordinate phase: 60 ℃, 2.5 hours, pressure-controlling was at 0.8Mpa;
In the 4th step, neutralization: add the Glacial acetic acid min. 99.5 that measures in advance at the precipitation still, be pressed into the intact material of etherificate and neutralize, heats up 80 ℃ and carry out precipitation, temperature rises to 102 ℃, the detection pH value be 8 o'clock be that precipitation finishes; Fill it up with 100 ℃ the tap water of crossing through the reverse osmosis apparatus processes at the precipitation still;
In the 5th step, centrifuge washing: the material in the 4th step is carried out spinning through horizontal spiral centrifuge, and separation of material is transferred to the washing still of filling it up with hot water in advance, carries out the washing of material;
In the 6th step, whiz: the material after the washing is conveyed into drying machine through horizontal spiral centrifuge, at 170 ℃ material is carried out drying, and the exsiccant material is pulverized the back packing.
What should explain at last is: obviously, the foregoing description only be for clearly the present invention is described and is done for example, and be not qualification to embodiment.For the those of ordinary skill in affiliated field, on the basis of above-mentioned explanation, can also make other multi-form variation or change.Here need not also can't give exhaustive to all embodiments.And conspicuous variation of being amplified out thus or change still are among protection scope of the present invention.
Claims (2)
1. the preparation method of a hydroxyethylmethyl-cellulose is characterized in that: said method for purified cotton as raw material, adopt oxyethane as etherifying agent, produce hydroxyethylmethyl-cellulose.
2. the preparation method of hydroxyethylmethyl-cellulose as claimed in claim 1 is characterized in that, the parts by weight of raw materials of preparation hydroxyethylmethyl-cellulose is provided as: toluene and isopropanol mixture are made solvent for 700～800 parts; 30～40 parts in water; 70～80 parts in sodium hydroxide, 80～85 parts of purified cottons, 20～28 parts in oxyethane; 80～90 parts of methyl chloride, 16～19 parts in Glacial acetic acid min. 99.5;
Concrete steps are:
The first step in reaction kettle, adds toluene and isopropanol mixture, water and sodium hydroxide, is warming up to 60～80 ℃, is incubated 20～40 minutes;
Second step, alkalization: above-mentioned material is cooled to 30～50 ℃, adds purified cotton; Carry out toluene and isopropanol mixture solvent spray; Be evacuated to-0.006Mpa, inflated with nitrogen carries out 3 displacements, replaces the laggard row alkalization that finishes; The alkalization condition is: alkalization time is 2 hours, and alkalization temperature is 30 ℃-50 ℃;
In the 3rd step, etherificate: alkalization finishes, and reaction kettle is evacuated to 0.05～0.07MPa, adds oxyethane and methyl chloride, keeps 30～50 minutes; The etherificate fs: 40～60 ℃, 1.0～2.0 hours, pressure-controlling was between 0.15-0.3Mpa; The etherificate subordinate phase: 60～90 ℃, 2.0～2.5 hours, pressure-controlling was between 0.4-0.8Mpa;
In the 4th step, neutralization: add the Glacial acetic acid min. 99.5 that measures in advance at the precipitation still, be pressed into the intact material of etherificate and neutralize, heat up 75～80 ℃ and carry out precipitation, temperature rises to 102 ℃, is that precipitation finishes when detecting pH value for 6-8; Fill it up with 90 ℃～100 ℃ the tap water of crossing through the reverse osmosis apparatus processes at the precipitation still;
In the 5th step, centrifuge washing: the material in the 4th step is carried out spinning through horizontal spiral centrifuge, and separation of material is transferred to the washing still of filling it up with hot water in advance, carries out the washing of material;
In the 6th step, whiz: the material after the washing is conveyed into drying machine through horizontal spiral centrifuge, at 150～170 ℃ material is carried out drying, and the exsiccant material is pulverized the back packing.
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| CN2012101451860A CN102690356A (en) | 2012-05-11 | 2012-05-11 | Preparation method of hydroxyl-ethyl methyl cellulose |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107108357A (en) * | 2015-01-12 | 2017-08-29 | 陶氏环球技术有限责任公司 | The methyl hydroxyethylcellulose as cement additire is used at high temperature |
| CN107964048A (en) * | 2018-01-04 | 2018-04-27 | 泸州北方化学工业有限公司 | A kind of coating process of hydrophobic associated ethoxyl cellulose |
| CN110981975A (en) * | 2019-11-28 | 2020-04-10 | 泸州北方纤维素有限公司 | Method for increasing viscosity of hydroxyethyl cellulose |
| CN112409498A (en) * | 2020-11-25 | 2021-02-26 | 泸州北方纤维素有限公司 | Preparation method of high-stability carboxymethyl hydroxyethyl cellulose |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101070351A (en) * | 2007-05-17 | 2007-11-14 | 湖州展望天明药业有限公司 | Polysubstituted radical cellulose composite ether and its preparing method |
| CN101955546A (en) * | 2009-07-15 | 2011-01-26 | 山东赫达股份有限公司 | Process for producing cellulose ether by directly separating and recovering diluent |
| CN102417542A (en) * | 2011-11-18 | 2012-04-18 | 新疆光大山河化工科技有限公司 | Method for producing hydroxypropyl methyl cellulose by using bamboo pulp |
-
2012
- 2012-05-11 CN CN2012101451860A patent/CN102690356A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101070351A (en) * | 2007-05-17 | 2007-11-14 | 湖州展望天明药业有限公司 | Polysubstituted radical cellulose composite ether and its preparing method |
| CN101955546A (en) * | 2009-07-15 | 2011-01-26 | 山东赫达股份有限公司 | Process for producing cellulose ether by directly separating and recovering diluent |
| CN102417542A (en) * | 2011-11-18 | 2012-04-18 | 新疆光大山河化工科技有限公司 | Method for producing hydroxypropyl methyl cellulose by using bamboo pulp |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107108357A (en) * | 2015-01-12 | 2017-08-29 | 陶氏环球技术有限责任公司 | The methyl hydroxyethylcellulose as cement additire is used at high temperature |
| CN107964048A (en) * | 2018-01-04 | 2018-04-27 | 泸州北方化学工业有限公司 | A kind of coating process of hydrophobic associated ethoxyl cellulose |
| CN110981975A (en) * | 2019-11-28 | 2020-04-10 | 泸州北方纤维素有限公司 | Method for increasing viscosity of hydroxyethyl cellulose |
| CN112409498A (en) * | 2020-11-25 | 2021-02-26 | 泸州北方纤维素有限公司 | Preparation method of high-stability carboxymethyl hydroxyethyl cellulose |
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Application publication date: 20120926 |