CN109957030A - A kind of preparation method of the hydroxypropyl methyl cellulose ether of high gelling temp - Google Patents
A kind of preparation method of the hydroxypropyl methyl cellulose ether of high gelling temp Download PDFInfo
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- CN109957030A CN109957030A CN201910286406.3A CN201910286406A CN109957030A CN 109957030 A CN109957030 A CN 109957030A CN 201910286406 A CN201910286406 A CN 201910286406A CN 109957030 A CN109957030 A CN 109957030A
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- hydroxypropyl methyl
- methyl cellulose
- cellulose ether
- temperature
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B11/00—Preparation of cellulose ethers
- C08B11/193—Mixed ethers, i.e. ethers with two or more different etherifying groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B11/00—Preparation of cellulose ethers
- C08B11/20—Post-etherification treatments of chemical or physical type, e.g. mixed etherification in two steps, including purification
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B15/00—Preparation of other cellulose derivatives or modified cellulose, e.g. complexes
- C08B15/005—Crosslinking of cellulose derivatives
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention discloses a kind of preparation methods of the hydroxypropyl methyl cellulose ether of high gelling temp, the specific steps are as follows: cellulose powder is added in alkalization kettle and alkalizes；Low-temp reaction after first temperature reaction carries out two step etherificates；It neutralizes and adjusts to realize and adjust acid；The cross-linked modifier of cellulose powder weight 1.0-4.0% is added after crushing to system, is stirred 10-30 minutes under conditions of 50-70 DEG C of temperature.This method can be prepared into the hydroxypropyl methyl cellulose ether of high-moisture-retention, and the homogeneity of gained hydroxypropyl methyl cellulose product is preferable, for water retentivity of mortar can be significantly improved in hot weather and high temperature mortar, present invention process does not need special consersion unit simultaneously, reaction condition is mild, and reaction process time-consuming is short.
Description
Technical field
It is fine that the present invention relates to the hydroxypropyl methyls of building additive preparation technical field more particularly to a kind of high gelling temp
Tie up the preparation method of plain ether.
Background technique
In dry-mixed mortar, cellulose ether is one of essential additive.When adding cellulose ether in dry-mixed mortar
Afterwards, the cement mortar after making mix has very high water-retaining property and good increasing stick effect, so that cement mortar is longer
Time keeps enough moisture content.In mix and work progress, water plays the work of lubricant and solvent between inorganic component
With, therefore thin layer mortar can just be combed, plastering mortar can just be paved with trowel.Sand in work progress simultaneously
Slurry, since water-retaining property increases after addition cellulose ether, hygroscopic wall or Ceramic Tiles do not need to prewet, while greatly
The workability and application property, promotion hydrated cementitious for improving mortar, effectively improve the adhesion strength of mortar product.
The water-retaining property of cellulose ether is the raising with temperature and is gradually reduced, especially the relatively low cellulose of gelling temp
Ether, during actual construction, dry powder and mortar are often constructed under conditions of high temperature (being higher than 35 DEG C), the base constructed at this time
The temperature of for example various walls itself of material is also higher, and (the especially wall of summer direct sunlight, temperature is even up to 60 DEG C -70
DEG C), there is situations such as carry out exterior wall putty in the case of solarization, plastering, tiling construction operation such as summer, there is also temperature in the north
Degree is high, the more adverse circumstances that relative humidity is low, wind speed is big.Due to the double influence of weather and substrate, make under the water retention of mortar
Drop causes dehydration too fast and influences the aquation of cement, and then makes the strength reduction of mortar, at the same application property and splitting resistance all by
To influence, thus the water retention property of cellulose ether at high temperature will be fully considered in this case.
The production of hydroxypropyl methyl cellulose HPMC has gas-solid method and two kinds of slurry process.HPMC production before mostly uses greatly silt
Can slurry processes be to make cellulose and lye, chloromethanes, propylene oxide etc. in paste-like as solvent using isopropanol, toluene unit
Reaction is come into full contact under state, completes alkalization, the etherificate of cellulose, Shi Changyue 12h.Slurry process reaction duration, water retention is high,
A large amount of solvent is used in production, needs to recycle after reaction to reduce cost, by-product is also difficult to control in reaction process.
Gas-solid method is divided into direct gas-solid method and vacuum gas-solid method again.The former is by cellulose after lye squeezes, with chloromethanes, epoxy
Propane directly reacts 3-6h at 45-90 DEG C, obtained various rank viscosity products；The latter be by cellulose alkalization squeeze after,
It puts into reactor under nitrogen protection, 1-3h is reacted at 40-60 DEG C of low temperature, then react 1-3h at 70-90 DEG C.Gas-solid method
Feature is that process is simple and fast, but the consumption of chloromethanes, propylene oxide is big, and product uniformity is poor, and product is unstable and gelling temp
It is low.
Summary of the invention
The purpose of the present invention is to solve disadvantages existing in the prior art, and a kind of hydroxyl of the high gelling temp proposed
The preparation method of propyl methocel ether, to effectively solve in the prior art that product uniformity is poor, product is unstable and solidifying
The low defect of glue temperature, when ensuring construction at high temperature, mortar still has the viscosity of good water-retaining property and mortar, to guarantee
Mortar strength is to prevent hollowing cracking picking.
To achieve the above object, the invention provides the following technical scheme: the invention discloses a kind of hydroxyls of high gelling temp
The preparation method of propyl methocel ether, the specific steps are as follows:
(1), it alkalizes
Cellulose powder is added in alkalization kettle and is alkalized；
(2), it is etherified
Low-temp reaction after first temperature reaction carries out two step etherificates；
(3), acid is adjusted
It neutralizes and adjusts to realize and adjust acid；
(4), it post-processes
The cross-linked modifier of cellulose powder weight 1.0-4.0% is added after crushing to system, is stirred under conditions of 50-70 DEG C of temperature
It mixes 10-30 minutes.
Preferably, the cellulose powder uses wood pulp powder in the step (1).
Preferably, the temperature of temperature reaction is 70-90 DEG C, reaction time 1-3h in the step (2), carry out
First step etherificate, then the temperature of low-temp reaction is 40-60 DEG C, reaction time 2-4h, carries out second step etherificate.
Preferably, in the step (3), added after etherificate the hot water of oxalic acid and temperature not less than 90 DEG C into
Row acidity or purity are adjusted, and continue stirring 10-30 minutes.
Preferably, in the step (4), the step of post-processing includes that the material after exchanging acid carries out wet-milling
It is broken, drying, crush again, in drying course use cross-linked modifier, it is 10-30 minutes cross-linking modified under the conditions of 50-70 DEG C.
Preferably, in the post-processing step, the wet feed after solid-liquid separation treatment is aqueous in the step (4)
Rate is 30%-65%, and treated that semi-finished product moisture content is 5%-10% for drying.
Preferably, the wood pulp powder is using one of Korean pine wood pulp, spruce pulp, birch wood pulp or a variety of timess
The combination of meaning ratio.
Preferably, the cross-linked modifier uses one of ethyl alcohol, propylene glycol, propylene glycol, urea or a variety of
The combination of arbitrary proportion.
Compared with the existing technology, technical effect of the invention and advantage are as follows:
Cellulose ether preparation method of the invention, alkalization, etherificate, tune acid and post-processing, this method including cellulose powder include
Alkalization, etherificate, adjust acid elution, be dry broken, the post-processing steps such as crosslinking are wherein after stirring according to acidity or whiteness
It is required that adding suitable oxalic acid and hot water of the temperature not less than 90 DEG C, continues stirring 10-30 minutes, clean 2-3 times, mesh
Internal salt is cleaned up, there is the salt of high concentration stronger hydrophily and polymer to compete and weaken polymer hydration
Effect, can reduce the gelling temp of hydroxypropyl methyl cellulose ether.
This method can be prepared into the hydroxypropyl methyl cellulose ether of high-moisture-retention, and gained hydroxypropyl methyl cellulose
The homogeneity of product is preferable, for that can significantly improve water retentivity of mortar, while this hair in hot weather and high temperature mortar
Bright technique does not need special consersion unit, and reaction condition is mild, and reaction process time-consuming is short.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, below in conjunction with specific embodiment, to this
Invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, not
For limiting the present invention.Based on the embodiments of the present invention, those of ordinary skill in the art are not before making creative work
Every other embodiment obtained is put, shall fall within the protection scope of the present invention.
Embodiment 1
The invention discloses a kind of preparation methods of the hydroxypropyl methyl cellulose ether of high gelling temp, the specific steps are as follows:
(1), it alkalizes
Cellulose powder is added in alkalization kettle and is alkalized；
(2), it is etherified
Low-temp reaction after first temperature reaction carries out two step etherificates；
(3), acid is adjusted
It neutralizes and adjusts to realize and adjust acid；
(4), it post-processes
The cross-linked modifier of cellulose powder weight 3% is added after crushing to system, is stirred 15 minutes under conditions of temperature 60 C.
In the step (1), the cellulose powder uses wood pulp powder.
In the step (2), the temperature of temperature reaction is 80 DEG C, reaction time 2h, carries out first step etherificate, then
The temperature of low-temp reaction is 50 DEG C, reaction time 3h, carries out second step etherificate.
In the step (3), oxalic acid is added after etherificate and 95 DEG C of hot water carries out acidity or purity is adjusted, is continued
Stirring 15 minutes, purpose clean up internal salt, and there is the salt of high concentration stronger hydrophily and polymer to compete
And weaken polymer hydration effect, the gelling temp of hydroxypropyl methyl cellulose ether can be reduced.
In the step (4), the step of post-processing includes that material after exchanging acid carries out broken wet-milling, drying, again
It crushes, cross-linked modifier is used in drying course, cross-linking modified 15 minutes under the conditions of 60 DEG C.
In the step (4), in the post-processing step, the wet feed moisture content after solid-liquid separation treatment is 45%,
Drying treated semi-finished product moisture content is 8%.
The wood pulp powder uses Korean pine wood pulp
The cross-linked modifier uses ethyl alcohol.
Embodiment 2
The invention discloses a kind of preparation methods of the hydroxypropyl methyl cellulose ether of high gelling temp, the specific steps are as follows:
(1), it alkalizes
Cellulose powder is added in alkalization kettle and is alkalized；
(2), it is etherified
Low-temp reaction after first temperature reaction carries out two step etherificates；
(3), acid is adjusted
It neutralizes and adjusts to realize and adjust acid；
(4), it post-processes
The cross-linked modifier of cellulose powder weight 2% is added after crushing to system, is stirred 30 minutes under conditions of 55 DEG C of temperature.
In the step (1), the cellulose powder uses wood pulp powder.
In the step (2), the temperature of temperature reaction is 90 DEG C, reaction time 2.5h, carries out first step etherificate, so
The temperature of low-temp reaction is 40 DEG C, reaction time 3.5h afterwards, carries out second step etherificate.
In the step (3), oxalic acid is added after etherificate and 90 DEG C of hot water carries out acidity or purity is adjusted, is continued
Stirring 15 minutes, purpose clean up internal salt, and there is the salt of high concentration stronger hydrophily and polymer to compete
And weaken polymer hydration effect, the gelling temp of hydroxypropyl methyl cellulose ether can be reduced.
In the step (4), the step of post-processing includes that material after exchanging acid carries out broken wet-milling, drying, again
It crushes, cross-linked modifier is used in drying course, cross-linking modified 30 minutes under the conditions of 50 DEG C.
In the step (4), in the post-processing step, the wet feed moisture content after solid-liquid separation treatment is 30%-
65%, drying treated semi-finished product moisture content is 5%-10%.
The wood pulp powder uses spruce pulp.
The cross-linked modifier uses propylene glycol.
Embodiment 3
The invention discloses a kind of preparation methods of the hydroxypropyl methyl cellulose ether of high gelling temp, the specific steps are as follows:
(1), it alkalizes
Cellulose powder is added in alkalization kettle and is alkalized；
(2), it is etherified
Low-temp reaction after first temperature reaction carries out two step etherificates；
(3), acid is adjusted
It neutralizes and adjusts to realize and adjust acid；
(4), it post-processes
The cross-linked modifier of cellulose powder weight 4.0% is added after crushing to system, stirs 30 under conditions of 50-70 DEG C of temperature
Minute.
In the step (1), the cellulose powder uses wood pulp powder.
In the step (2), the temperature of temperature reaction is 70 DEG C, reaction time 2h, carries out first step etherificate, then
The temperature of low-temp reaction is 60 DEG C, reaction time 4h, carries out second step etherificate.
In the step (3), oxalic acid is added after etherificate and 90 DEG C of hot water carries out acidity or purity is adjusted, is continued
Stirring 30 minutes, purpose clean up internal salt, and the salt of high concentration has stronger hydrophily and polymer competing
It strives and weakens polymer hydration effect, the gelling temp of hydroxypropyl methyl cellulose ether can be reduced.
In the step (4), the step of post-processing includes that material after exchanging acid carries out broken wet-milling, drying, again
It crushes, cross-linked modifier is used in drying course, cross-linking modified 30 minutes under the conditions of 60 DEG C.
In the step (4), in the post-processing step, the wet feed moisture content after solid-liquid separation treatment is 45%,
Drying treated semi-finished product moisture content is 8%.
The wood pulp powder uses birch wood pulp.
The cross-linked modifier uses urea.
Table 1 is the performance that the hydroxypropyl methyl cellulose ether for the high gelling temp that embodiment 1,2,3 is prepared carries out
Detection, testing result are as follows:
As can be seen from the above table, the hydroxypropyl methyl cellulose ether of the high gelling temp obtained using preparation method of the present invention is sticked
Degree reduces, and water retention, light transmittance and gelling temp greatly improve, in addition, the product obtained through preparation method of the present invention is than tradition
The product that technique obtains is more suitable for that high temperature dwell is aqueous, the loss of mortar Free water when reducing high temperature, so as to avoid by
The quality problems caused by water loss is too fast.
Finally, it should be noted that the foregoing is only a preferred embodiment of the present invention, it is not intended to restrict the invention,
Although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art, still may be used
To modify the technical solutions described in the foregoing embodiments or equivalent replacement of some of the technical features,
All within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in of the invention
Within protection scope.
Claims (8)
1. a kind of preparation method of the hydroxypropyl methyl cellulose ether of high gelling temp, it is characterised in that: specific step is as follows:
(1), it alkalizes
Cellulose powder is added in alkalization kettle and is alkalized；
(2), it is etherified
Low-temp reaction after first temperature reaction carries out two step etherificates；
(3), acid is adjusted
It neutralizes and adjusts to realize and adjust acid；
(4), it post-processes
The cross-linked modifier of cellulose powder weight 1.0-4.0% is added after crushing to system, is stirred under conditions of 50-70 DEG C of temperature
It mixes 10-30 minutes.
2. a kind of preparation method of the hydroxypropyl methyl cellulose ether of high gelling temp according to claim 1, feature
Be: in the step (1), the cellulose powder uses wood pulp powder.
3. a kind of preparation method of the hydroxypropyl methyl cellulose ether of high gelling temp according to claim 1, feature
Be: in the step (2), the temperature of temperature reaction is 70-90 DEG C, reaction time 1-3h, carries out first step etherificate, so
The temperature of low-temp reaction is 40-60 DEG C, reaction time 2-4h afterwards, carries out second step etherificate.
4. a kind of preparation method of the hydroxypropyl methyl cellulose ether of high gelling temp according to claim 1, feature
It is: in the step (3), the hot water of oxalic acid and temperature not less than 90 DEG C is added after etherificate and carries out acidity or purity
It adjusts, continues stirring 10-30 minutes.
5. a kind of preparation method of the hydroxypropyl methyl cellulose ether of high gelling temp according to claim 1, feature
Be: in the step (4), the step of post-processing includes that material after exchanging acid carries out that wet-milling is broken, drying, again powder
It is broken, cross-linked modifier is used in drying course, it is 10-30 minutes cross-linking modified under the conditions of 50-70 DEG C.
6. a kind of preparation method of the hydroxypropyl methyl cellulose ether of high gelling temp according to claim 1 or 5, special
Sign is: in the step (4), in the post-processing step, the wet feed moisture content after solid-liquid separation treatment is 30%-
65%, drying treated semi-finished product moisture content is 5%-10%.
7. a kind of preparation method of the hydroxypropyl methyl cellulose ether of high gelling temp according to claim 2, feature
Be: the wood pulp powder uses the group of one of Korean pine wood pulp, spruce pulp, birch wood pulp or a variety of arbitrary proportions
It closes.
8. a kind of preparation method of the hydroxypropyl methyl cellulose ether of high gelling temp according to claim 1 or 5, special
Sign is: the cross-linked modifier is using one of ethyl alcohol, propylene glycol, propylene glycol, urea or a variety of arbitrary proportions
Combination.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910286406.3A CN109957030A (en) | 2019-04-10 | 2019-04-10 | A kind of preparation method of the hydroxypropyl methyl cellulose ether of high gelling temp |
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| CN201910286406.3A CN109957030A (en) | 2019-04-10 | 2019-04-10 | A kind of preparation method of the hydroxypropyl methyl cellulose ether of high gelling temp |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105111317A (en) * | 2015-08-28 | 2015-12-02 | 广东龙湖科技股份有限公司 | Preparation method of cellulose ether and cellulose ether obtained in same |
| CN106939052A (en) * | 2017-03-24 | 2017-07-11 | 山东滕新材料股份有限公司 | A kind of preparation method of cellulose ether |
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2019
- 2019-04-10 CN CN201910286406.3A patent/CN109957030A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105111317A (en) * | 2015-08-28 | 2015-12-02 | 广东龙湖科技股份有限公司 | Preparation method of cellulose ether and cellulose ether obtained in same |
| CN106939052A (en) * | 2017-03-24 | 2017-07-11 | 山东滕新材料股份有限公司 | A kind of preparation method of cellulose ether |
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Application publication date: 20190702 |