CN109517075A - A kind of method for preparing hydroxypropylmethylcellulose and product - Google Patents
A kind of method for preparing hydroxypropylmethylcellulose and product Download PDFInfo
- Publication number
- CN109517075A CN109517075A CN201811402778.XA CN201811402778A CN109517075A CN 109517075 A CN109517075 A CN 109517075A CN 201811402778 A CN201811402778 A CN 201811402778A CN 109517075 A CN109517075 A CN 109517075A
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- Prior art keywords
- hydroxypropyl methyl
- methyl cellulose
- granulation
- water
- product
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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
-
- 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
- C08B11/22—Isolation
-
- 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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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Materials Engineering (AREA)
- 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 method for preparing hydroxypropylmethylcellulose and products, the described method comprises the following steps: (1) hydroxypropyl methyl cellulose crude product is made in etherified react；(2) etherification reaction used solvent in the process is recycled through precipitation；(3) hydroxypropyl methyl cellulose crude product and water are separated through filtration washing and removes the impurity in hydroxypropyl methyl cellulose crude product；(4) crosslinking Treatment is carried out to the material spray glyoxal water solution after filtration washing；(5) material after crosslinking Treatment enters pelletizer progress extrusion granulation, and cools down to the material after granulation；(6) material after granulation is pre-milled, drying, crushing obtain hydroxypropyl methyl cellulose product.The present invention can obtain the hydroxypropyl methyl cellulose of long delay dissolution time.
Description
Technical field
The invention belongs to field of fine chemical, and in particular to a kind of method for preparing hydroxypropylmethylcellulose and product.
Background technique
Hydroxypropyl methyl cellulose is a kind of nonionic cellulose compound ether.It is it is a kind of it is semi-synthetic, sluggish,
The polymer of viscoelasticity is often used as lubrication section in ophthalmology, and or auxiliary material or excipients are served as in oral drugs, be common in each
The different types of commodity of kind.As food additives, hydroxypropyl methylcellulose may act as following role: emulsifier, thickener, suspension
The substitute of agent and animal gelatin.
Conventional hydroxypropyl methyl cellulose product only disperses in the hot water, is insoluble, dissolves rapidly in cold water.For building
The hydroxypropyl methyl cellulose product of material industry is usually delayed dissolved type, i.e., first disperses in cold water, is redissolved, from add water to
This period, that is, delayed dissolved time of dispersion, dissolution.
Delayed dissolved cellulose is prepared at present to be crosslinked hydroxypropyl methyl cellulose product usually using dialdehyde solution
Processing can get product of the delayed dissolved time within 5 minutes, but be difficult to obtain long delay dissolution time (when delayed dissolved
Between at 5-10 minutes) hydroxypropyl methyl cellulose product.
Summary of the invention
The object of the present invention is to provide a kind of method for preparing hydroxypropylmethylcellulose and products, to overcome in the prior art
Short problem of existing hydroxypropyl methyl cellulose delayed dissolved time.
To achieve the goals above, one aspect of the present invention provides a kind of method for preparing hydroxypropylmethylcellulose, packet
Include following steps: (1) hydroxypropyl methyl cellulose crude product is made in etherified react；(2) etherification reaction is recycled through precipitation
Used solvent in the process；(3) hydroxypropyl methyl cellulose crude product and water are separated through filtration washing and removes hydroxypropyl first
Impurity in base cellulose crude product；(4) crosslinking Treatment is carried out to the material spray glyoxal water solution after filtration washing；
(5) material after crosslinking Treatment enters pelletizer progress extrusion granulation, and cools down to the material after granulation；(6) it will be granulated
Material afterwards is pre-milled, dry, crushing obtains hydroxypropyl methyl cellulose product.
Preferably, in step (4), the concentration of glyoxal water solution is 3%-10%.
Preferably, in step (5), the pelletizer uses screw extruder.
Preferably, in step (5), increase the water content of material by granulation process.
Preferably, in step (5), the material after granulation is cooled down using -20~-5 DEG C of water at low temperature.
Preferably, the water at low temperature uses hypothermic saline.
Another aspect of the present invention provides a kind of hydroxypropyl methyl cellulose product being prepared by above-mentioned method.
Using the technical solution of aforementioned aspect of the present invention, the hydroxypropyl methyl fiber of long delay dissolution time can be obtained
Element.
Detailed description of the invention
Fig. 1 is the flow chart of the method for preparing hydroxypropylmethylcellulose of one embodiment of the present invention.
Specific embodiment
Technical solution of the present invention will be clearly and completely described below, it is clear that described embodiment is this hair
Bright a part of the embodiment, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not having
Every other embodiment obtained under the premise of creative work is made, shall fall within the protection scope of the present invention.
The present invention provides a kind of hydroxypropyl methyl of long delay dissolution time (the delayed dissolved time was at 5-10 minutes) fibres
Tie up plain preparation method.This method is also sharp in addition to using glyoxal solution to carry out crosslinking Treatment to hydroxypropyl methyl cellulose product
Increase material moisture with granulation process, obtain the product of high bulk density by water at low temperature (such as -15 DEG C) cooling, from
And obtain the hydroxypropyl methyl cellulose product of long delay dissolution time (the delayed dissolved time was at 5-10 minutes).
Fig. 1 is the flow chart of the method for preparing hydroxypropylmethylcellulose of one embodiment of the present invention.As shown in Figure 1,
The method of the present invention includes the following steps:
(1) hydroxypropyl methyl cellulose crude product is made in etherified react.
Etherification reaction is for example including alkali, cotton powder, etherifying agent, solvent.
(2) through solvent used in precipitation recycling etherification reaction process.
Solvent after precipitation sends to solvent recovering system.
(3) miscellaneous in the separation and removal product through filtration washing to realize hydroxypropyl methyl cellulose product and water
Matter.
Water and impurity after filtration washing go to waste water treatment system.
(4) aqueous solution (glyoxal concentration is, for example, 3%-10%) of washed filtered material spray glyoxal carries out
Crosslinking Treatment.
(5) material enters pelletizer (screw extruder) progress extrusion granulation to improve compaction rate, pelletizer use -20
~-5 DEG C of water at low temperature is cooled down, to ensure granulation outcome.
Here water at low temperature can be hypothermic saline.
(6) be granulated after material it is pre-milled, drying, crush obtain hydroxypropyl methyl cellulose product.
Embodiment 1
10~12 mass fraction organic solvents, several pieces alkali of 0.5~1.5 mass parts and a certain amount of are added into reaction kettle
Water is warming up to 70 DEG C~90 DEG C and keeps the temperature 1~2h.Reaction kettle is cooled to 20 DEG C~40 DEG C, 1 mass fraction cotton fiber is added,
Alkalize 1~2h.0.2~1 mass fraction propylene oxide and 0.5~2 mass fraction monochloro methane is added, is warming up to 50 DEG C~90 DEG C
5~10h of lower reaction.Thus hydroxypropyl methyl cellulose crude product is made.
Distillation, recycling design.Slurry separates through filtration washing realization water and product and removes impurity.Hydroxypropyl methyl fiber
Plain filter cake spray glyoxal water solution (concentration 3%-10%) carries out crosslinking Treatment.Material enters pelletizer (screw extruder),
The water at low temperature that -20~-5 DEG C of pelletizer use is cooled down, and more closely knit material is obtained after being granulated.Material is pre-milled,
Drying obtains the hydroxypropyl methyl cellulose product of long delay dissolution time after crushing.
Embodiment 2
10~12 mass fraction organic solvents, several pieces alkali of 0.5~1.5 mass parts and a certain amount of are added into reaction kettle
Water is warming up to 70 DEG C~90 DEG C and keeps the temperature 1~2h.Reaction kettle is cooled to 20 DEG C~40 DEG C, 1 mass fraction cotton fiber is added,
Alkalize 1~2h.0.2~1 mass fraction propylene oxide and 0.5~2 mass fraction monochloro methane is added, is warming up to 50 DEG C~90 DEG C
5~10h of lower reaction.Thus hydroxypropyl methyl cellulose crude product is made.
Distillation, recycling design.Slurry separates through filtration washing realization water and product and removes impurity.Hydroxypropyl methyl fiber
Plain filter cake spray glyoxal water solution (concentration 3%-10%) carries out crosslinking Treatment.Material enters pelletizer (screw extruder),
The water at low temperature that -20~-5 DEG C of pelletizer use is cooled down, and more closely knit material is obtained after being granulated.Material is pre-milled,
Drying obtains the hydroxypropyl methyl cellulose product of long delay dissolution time after crushing.
The hydroxypropyl methyl cellulose product that through the foregoing embodiment 1 and embodiment 2 obtain is analyzed to obtain following
The result of table 1.
Table 1 analyzes result
From the analysis result of table 1 it is found that the hydroxypropyl methyl cellulose that the present invention can prepare long delay dissolution time produces
Product.
Obviously, the above embodiments are merely examples for clarifying the description, and does not limit the embodiments.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of variation or
It changes.There is no necessity and possibility to exhaust all the enbodiments.And it is extended from this it is obvious variation or
It changes still within the protection scope of the invention.
Claims (7)
1. a kind of method for preparing hydroxypropylmethylcellulose, which comprises the following steps:
(1) hydroxypropyl methyl cellulose crude product is made in etherified react；
(2) etherification reaction used solvent in the process is recycled through precipitation；
(3) hydroxypropyl methyl cellulose crude product and water are separated through filtration washing and removed in hydroxypropyl methyl cellulose crude product
Impurity；
(4) crosslinking Treatment is carried out to the material spray glyoxal water solution after filtration washing；
(5) material after crosslinking Treatment enters pelletizer progress extrusion granulation, and cools down to the material after granulation；
(6) material after granulation is pre-milled, drying, crushing obtain hydroxypropyl methyl cellulose product.
2. the method according to claim 1, wherein the concentration of glyoxal water solution is 3%- in step (4)
10%.
3. method according to claim 1 or 2, which is characterized in that in step (5), the pelletizer is squeezed using screw rod
Machine out.
4. method according to any one of claim 1-3, which is characterized in that in step (5), increased by granulation process
Add the water content of material.
5. method according to any of claims 1-4, which is characterized in that in step (5), use -20~-5 DEG C
Water at low temperature the material after granulation is cooled down.
6. according to the method described in claim 5, it is characterized in that, the water at low temperature uses hypothermic saline.
7. a kind of hydroxypropyl methyl cellulose product being prepared by method of any of claims 1-6.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811402778.XA CN109517075A (en) | 2018-11-22 | 2018-11-22 | A kind of method for preparing hydroxypropylmethylcellulose and product |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811402778.XA CN109517075A (en) | 2018-11-22 | 2018-11-22 | A kind of method for preparing hydroxypropylmethylcellulose and product |
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| Publication Number | Publication Date |
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| CN109517075A true CN109517075A (en) | 2019-03-26 |
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| CN201811402778.XA Pending CN109517075A (en) | 2018-11-22 | 2018-11-22 | A kind of method for preparing hydroxypropylmethylcellulose and product |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101830990A (en) * | 2010-05-08 | 2010-09-15 | 山东一滕化工有限公司 | Instant hydroxypropyl methyl cellulose ether and preparation method thereof |
| CN103561728A (en) * | 2011-04-06 | 2014-02-05 | 陶氏环球技术有限责任公司 | Process for producing cellulose derivatives of high bulk density, good flowability and improved dispersibility in cold water |
-
2018
- 2018-11-22 CN CN201811402778.XA patent/CN109517075A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101830990A (en) * | 2010-05-08 | 2010-09-15 | 山东一滕化工有限公司 | Instant hydroxypropyl methyl cellulose ether and preparation method thereof |
| CN103561728A (en) * | 2011-04-06 | 2014-02-05 | 陶氏环球技术有限责任公司 | Process for producing cellulose derivatives of high bulk density, good flowability and improved dispersibility in cold water |
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| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB02 | Change of applicant information |
Address after: 646605 High Dam in Longmatan District, Luzhou City, Sichuan Province Applicant after: North Tianpu Cellulose Co., Ltd. Address before: 646605 High Dam in Longmatan District, Luzhou City, Sichuan Province Applicant before: Northern Tian Pu Chemical Co., Ltd. |
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| CB02 | Change of applicant information | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190326 |
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| RJ01 | Rejection of invention patent application after publication |