CN107129540A - The Green production method of hydroxypropyl methylcellulose - Google Patents
The Green production method of hydroxypropyl methylcellulose Download PDFInfo
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- CN107129540A CN107129540A CN201610122501.6A CN201610122501A CN107129540A CN 107129540 A CN107129540 A CN 107129540A CN 201610122501 A CN201610122501 A CN 201610122501A CN 107129540 A CN107129540 A CN 107129540A
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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
- C08B1/00—Preparatory treatment of cellulose for making derivatives thereof, e.g. pre-treatment, pre-soaking, activation
- C08B1/08—Alkali cellulose
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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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Abstract
The present invention relates to the Green production method of hydroxypropyl methylcellulose.The present invention uses toluene-isopropanol-water mixed system, purified cotton after crushing obtains HPMC crude products in the presence of alkali with expoxy propane, chloromethanes reaction production, the HPMC crude products are mixed with toluene-isopropanol-water mixed system, need, by solvent recovery, then to post-process HPMC crude products.The present invention drains into the mixed system after neutralization in precipitation kettle, and top hot water is added while stirring, continuously stirs more than 10 minutes, then static more than 20 minutes, forms solid-liquid-gas three phase；Most liquid solvent is reclaimed from the discharge of pipes of precipitation kettle waist position；The fraction liquid solvent and gaseous solvent of residual are reclaimed through distilling approach again.The scheme directly distilled compared with prior art, the present invention significantly reduces energy consumption, and the purity of HPMC crude products is higher, also reduces later stage HPMC intractability.
Description
Technical field
The present invention relates to the Green production method of the production method of hydroxypropyl methylcellulose, more particularly to hydroxypropyl methylcellulose.
Background technology
Domestic HPMC production largely uses toluene-isopropanol-water mixed system, and the purified cotton after crushing is in alkali
Effect is lower to be produced with expoxy propane, chloromethanes reaction；The mixed gas of toluene, isopropanol can be produced in production process；Chloromethane
The side reaction product of alkane, expoxy propane；Contain sodium chloride and sodium acetate in waste water.At present, domestic HPMC production technology is basic
On be all：One step slurry process, processing step substantially is as follows：（1）, pretreatment：Purified cotton is made to the purified cotton of 60-100 mesh
Powder；（2）Alkalization：By purified cotton powder in the dispersion of 8-10 times of mixed solvent, and alkali reaction, generate alkalinized celluloses；
（3）, etherificate：Etherification reaction occurs for alkalinized celluloses and expoxy propane, chloromethanes, HPMC crude products is made, the crude product is dispersed in molten
In agent system；（4）, neutralize：After reaction terminates, remaining alkali is neutralized with acid, the pH value of product is reached defined requirement；
（5）, solvent recovery：By the mixed system heating after neutralization, by condensation, the mixed solvent of cooling recovery system, after recovery
Solvent repetitive cycling is utilized；（6）, post processing：Mixture after precipitation passes through horizontal decanter centrifuge, centrifuges, and is passing through
Granulation, dry, mixing, packaging turn into final products.This method side reaction degree is low, product yield is high；But in solvent recovery
There is the problem of high energy consumption is reclaimed in evaporation in link.
The content of the invention
The invention solves the problems that above mentioned problem, so as to provide a kind of Green production method of hydroxypropyl methylcellulose.
Technical proposal that the invention solves the above-mentioned problems is as follows：
The Green production method of hydroxypropyl methylcellulose, comprises the following steps：
1）, pretreatment：Purified cotton is broken into the purified cotton block of about 1-3 centimetres of diameter by opener, subsequently into pulverizer,
Through high energy shear milling into 60-100 mesh purified cotton powder；
2）, alkalization：Purified cotton powder after crushing is in the dispersion of the mixed solvent of 8-10 times of toluene-isopropanol-water, and alkali
Generation alkalinization, alkali cellulose of the generation with reactivity；
3）, etherificate：Etherification reaction occurs for alkali cellulose and expoxy propane, chloromethanes, by reaction temperature, reaction time and matching somebody with somebody
The control of side, to adjust the height of methoxyl group and hydroxypropyl substitution value, is controlled by the content to oxidant in system environment, and
The viscosity height for selecting to adjust product of purified cotton raw materials；
4）, neutralize：After reaction terminates, remaining alkali is neutralized with acid；
5）, precipitation：Mixed system after neutralization is drained into precipitation kettle, the reinforcing that precipitation kettle is opened when discharge starts is stirred
Mix, top hot water is added while stirring, continuously stir more than 10 minutes, then static more than 20 minutes, form solid-liquid-gas three phase；Will
Most liquid solvent is reclaimed from the discharge of pipes of precipitation kettle waist position；Again by the liquid solvent and gaseous solvent of part through distillation
Approach is reclaimed；
6）, post processing：Mixture after precipitation passes through horizontal decanter centrifuge, centrifuges, then by granulating, drying, mix,
Packaging turns into final products.
It is used as the preferred of above-mentioned technical proposal, step 5）In, reinforcing stirring, the reinforcing stirring are carried out by stirring structure
It is that one-level blade is set up on the agitating shaft of precipitation kettle, and blade up and down is connected into the frame knot to be formed using connecting rod
Structure.
It is used as the preferred of above-mentioned technical proposal, step 5）In, the addition of hot water is 0.6~1.0 times of solvent volume.
It is used as the preferred of above-mentioned technical proposal, step 5）In, liquid solvent is imported after the pipeline discharge of precipitation kettle waist position
Into bypass channel tank, and after through static layering, water is discharged.
It is used as the preferred of above-mentioned technical proposal, step 5）In, after hot water is added, to prevent temperature to be less than 100 DEG C.
It is used as the preferred of above-mentioned technical proposal, step 5）In, before solvent discharge, pneumatic operated valve need to be first opened, then open on visor
Square ball valve.
It is used as the preferred of above-mentioned technical proposal, step 5）In, during solvent discharge, solvent tube valve is first opened, with a small portion
Point solvent recoil delivery pipe and pneumatic operated valve, it is appropriate it is static once.
It is used as the preferred of above-mentioned technical proposal, step 5）In, during solvent discharge, start solvent pump, then a little opening solvent
The situation of recycling design in pipe ball valve, observation visor, solvent clear, then big solvent pipe ball valve is gradually opened, solvent is increased
Reclaim speed.
It is used as the preferred of above-mentioned technical proposal, step 5）In, when solvent discharge is completed, solvent pump is closed down, then use a small amount of height
Position groove solvent suitably recoils solvent discharge pipe and pneumatic operated valve, is then shut off each valve.
It is used as the preferred of above-mentioned technical proposal, step 5）In, during solvent discharge, if solvent is opaque, containing a large amount of materials,
And continuously, then must terminate solvent discharge in time, and closing valve and stop solvent pump, it is then appropriate with a small amount of head tank solvent
Recoil, then appropriate static a period of time, then discharge.
The invention has the advantages that：
1st, the present invention after completion of the reaction, is first heating water, and stirs simultaneously, then by precipitation, makes solvent and reactants separate, so
Most liquid solvent is discharged by the pipe positioned at precipitation kettle waist position afterwards, remaining fraction solvent then passes through routine
Distillation approach is reclaimed；The scheme directly distilled compared with prior art, significantly reduces energy consumption；
2nd, obtained reactant is reclaimed using the method for the present invention because heating water take part in separation process so that material of the invention
The HPMC that method is produced compared with prior art, the purity of crude product is higher, reduces later stage HPMC intractability；
3rd, the present invention is in solvent recovery, due to adding hot water, therefore, it is necessary to which water is passed through into bypass channel tank after solvent recovery
Separate, so as to obtain the repeatable solvent utilized, the recovery utilization rate of solvent has reached more than 90%；
4th, solvent reclaiming rate of the invention is high, and in solvent recovery, has used substantial amounts of hot water greatly to dilute reaction
The concentration of product and solvent, therefore in final waste discharge, COD content is very low, has reached environmental protection standard, can directly arrange
Put.
Embodiment
Present embodiment is only explanation of the invention, is not limitation of the present invention.People in the art
Member's any change for being made after the specification of the present invention has been read, as long as in the range of claims, all will be by
The protection of Patent Law.
Embodiment one
1st, the pretreatment of cellulosic material
Purified cotton is broken into the purified cotton block of about 1-3 centimetres of diameter by opener, subsequently into pulverizer, through high speed shear
It is ground into the purified cotton powder of 60-100 mesh.
Existing HPMC production technologies are all by cellulosic material --- purified cotton, by shredding, crushing, cyclonic separation,
Several steps such as bag-type dusting packaging complete the preprocessing process of cellulosic material.
The primary pollution source of this technical process is dust pollution, and the main source of dust is the cellulose that crushing process is produced
Molecule, causes the dust pollution of air.
The dust generation opened bag and crush two steps of whole pretreating process process is less.Shredding step, is by hand
The sheet purified cotton that work opens after bag is placed on opener, is torn into 1-3cm loose fritter.The step is due to charging
It is usually unlimited so be easier to produce dust, and the equipment of different manufacturers, the sealing of feed arrangement is variant, plus
The difference of upper operative, producing the degree and quantity of dust also has larger difference.
2nd, alkalization, etherificate, solvent recovery, washing process
This process is the main stage of reaction of HPMC productions, is also the generation link of pollution sources mainly.
Technical process is as follows：
Purified cotton powder after crushing is in the dispersion of 8-10 times of mixed solvent, and alkalinization occurs for alkali, and generation has anti-
Answer the alkali cellulose of activity.
Etherificate：Etherification reaction occurs for alkali cellulose and expoxy propane, chloromethanes, by reaction temperature, the reaction time and
The control of formula, to adjust the height of methoxyl group and hydroxypropyl substitution value, is controlled by the content to oxidant in system environment,
The viscosity height of product is adjusted with the selection of purified cotton raw materials.
Neutralize：After reaction terminates, remaining alkali is neutralized with acid.
Precipitation：Mixed system after neutralization is drained into precipitation kettle, the reinforcing that precipitation kettle is opened when discharge starts is stirred
Mix, top hot water is added while stirring, continuously stir more than 10 minutes, then static more than 20 minutes, form solid-liquid-gas three phase；Will
Most liquid solvent is reclaimed from the discharge of pipes of precipitation kettle waist position；Again by the liquid solvent and gaseous solvent of part through distillation
Approach is reclaimed.
In whole process, solvent recovery is emphasis.Organic solvent is not only the means of production of preciousness, and deals with improperly just
Environment can be polluted, pollution water and soil and air.
In the prior art, it is to use direct distillation to reclaim organic solvent, so handles energy consumption higher.
In the present invention, water after completion of the reaction, is first being heated, and is being stirred simultaneously, then by precipitation, is making solvent and reactant point
From then by discharging most liquid solvent positioned at the pipe of precipitation kettle waist, remaining fraction solvent then passes through
Conventional distillation approach is reclaimed；The scheme directly distilled compared with prior art, significantly reduces energy consumption.
The material balance of process is as follows：Solvent balance：With the 7000 kilograms of solvent calculating that feed intake
Chloromethanes is balanced：With the 600 kilograms of chloromethanes calculating that feed intake
Expoxy propane is balanced：To feed intake, 180 kg ethylene propane are calculated
3rd, HPMC post processing
Post processing：Mixture after precipitation passes through horizontal decanter centrifuge, centrifuges, then by granulation, dry, mixing, bag
Dress up as final products.
HPMC aftertreatment technologys have been mature on the whole now, so also progressively having obtained manufacturing enterprise in terms of ambient influnence
Attention, while the control of dust, new economic benefit is also created to enterprise.
Claims (10)
1. the Green production method of hydroxypropyl methylcellulose, comprises the following steps：
1）, pretreatment：Purified cotton is broken into the purified cotton block of about 1-3 centimetres of diameter by opener, subsequently into pulverizer,
Through high energy shear milling into 60-100 mesh purified cotton powder；
2）, alkalization：Purified cotton powder after crushing is in the dispersion of the mixed solvent of 8-10 times of toluene-isopropanol-water, and alkali
Generation alkalinization, alkali cellulose of the generation with reactivity；
3）, etherificate：Etherification reaction occurs for alkali cellulose and expoxy propane, chloromethanes, by reaction temperature, reaction time and matching somebody with somebody
The control of side, to adjust the height of methoxyl group and hydroxypropyl substitution value, is controlled by the content to oxidant in system environment, and
The viscosity height for selecting to adjust product of purified cotton raw materials；
4）, neutralize：After reaction terminates, remaining alkali is neutralized with acid；
5）, precipitation：Mixed system after neutralization is drained into precipitation kettle, the reinforcing that precipitation kettle is opened when discharge starts is stirred
Mix, top hot water is added while stirring, continuously stir more than 10 minutes, then static more than 20 minutes, form solid-liquid-gas three phase；Will
Most liquid solvent is reclaimed from the discharge of pipes of precipitation kettle waist position；Again by the liquid solvent and gaseous solvent of part through distillation
Approach is reclaimed；
6）, post processing：Mixture after precipitation passes through horizontal decanter centrifuge, centrifuges, then by granulating, drying, mix,
Packaging turns into final products.
2. the Green production method of hydroxypropyl methylcellulose according to claim 1, it is characterised in that：Step 5）In, pass through
Stirring structure carries out reinforcing stirring, and the reinforcing stirring is that one-level blade is set up on the agitating shaft of precipitation kettle, and uses connection
Blade up and down is connected the closed-in construction to be formed by bar.
3. the Green production method of hydroxypropyl methylcellulose according to claim 2, it is characterised in that：Step 5）In, hot water
Addition be 0.6~1.0 times of solvent volume.
4. the Green production method of hydroxypropyl methylcellulose according to claim 1, it is characterised in that：Step 5）In, liquid
Solvent is imported into bypass channel tank after the pipeline discharge of precipitation kettle waist position, and after through static layering, water is discharged.
5. the Green production method of hydroxypropyl methylcellulose according to claim 1, it is characterised in that：Step 5）In, hot water
After addition, temperature is prevented to be less than 100 DEG C.
6. the Green production method of hydroxypropyl methylcellulose according to claim 1, it is characterised in that：Step 5）In, solvent
Before discharge, pneumatic operated valve need to be first opened, then open ball valve above visor.
7. the Green production method of hydroxypropyl methylcellulose according to claim 1, it is characterised in that：Step 5）In, solvent
During discharge, first to open solvent tube valve, be recoiled delivery pipe and pneumatic operated valve with sub-fraction solvent, it is appropriate it is static once.
8. the Green production method of hydroxypropyl methylcellulose according to claim 1, it is characterised in that：Step 5）In, solvent
During discharge, start solvent pump, then a little situation for opening recycling design in solvent pipe ball valve, observation visor, solvent clear
, then big solvent pipe ball valve is gradually opened, solvent recovery speed is increased.
9. the Green production method of hydroxypropyl methylcellulose according to claim 1, it is characterised in that：Step 5）In, solvent
When discharge is completed, solvent pump is closed down, then suitably recoiled with a small amount of head tank solvent solvent discharge pipe and pneumatic operated valve, it is then shut off each
Valve.
10. the Green production method of hydroxypropyl methylcellulose according to claim 1, it is characterised in that：Step 5）In, solvent
During discharge, if solvent is opaque, containing a large amount of materials, and continuously, then must terminate solvent discharge in time, closing valve and
Stop solvent pump, then suitably recoiled with a small amount of head tank solvent, then appropriate static a period of time, then discharge.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610122501.6A CN107129540B (en) | 2016-03-04 | 2016-03-04 | The Green production method of hydroxypropyl methylcellulose |
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| CN201610122501.6A CN107129540B (en) | 2016-03-04 | 2016-03-04 | The Green production method of hydroxypropyl methylcellulose |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108129575A (en) * | 2017-12-13 | 2018-06-08 | 浙江中维药业股份有限公司 | A kind of preparation method of low viscosity pharmaceutic adjuvant plant capsule hydroxypropyl methylcellulose |
| CN109337116A (en) * | 2018-11-22 | 2019-02-15 | 北方天普化工有限公司 | A kind of hydroxypropyl methyl cellulose method for recovering solvents |
| CN117229425A (en) * | 2023-10-16 | 2023-12-15 | 河北双牛建材纤维素有限公司 | Method for preparing high-purity hydroxypropyl methyl cellulose |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101260158A (en) * | 2008-04-14 | 2008-09-10 | 浙江中维药业有限公司 | Method for preparing hydroxypropylmethylcellulose |
| CN102603899A (en) * | 2012-02-24 | 2012-07-25 | 邸勇 | Process for producing low-substituted hydroxypropyl cellulose |
-
2016
- 2016-03-04 CN CN201610122501.6A patent/CN107129540B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101260158A (en) * | 2008-04-14 | 2008-09-10 | 浙江中维药业有限公司 | Method for preparing hydroxypropylmethylcellulose |
| CN102603899A (en) * | 2012-02-24 | 2012-07-25 | 邸勇 | Process for producing low-substituted hydroxypropyl cellulose |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108129575A (en) * | 2017-12-13 | 2018-06-08 | 浙江中维药业股份有限公司 | A kind of preparation method of low viscosity pharmaceutic adjuvant plant capsule hydroxypropyl methylcellulose |
| CN109337116A (en) * | 2018-11-22 | 2019-02-15 | 北方天普化工有限公司 | A kind of hydroxypropyl methyl cellulose method for recovering solvents |
| CN117229425A (en) * | 2023-10-16 | 2023-12-15 | 河北双牛建材纤维素有限公司 | Method for preparing high-purity hydroxypropyl methyl cellulose |
| CN117229425B (en) * | 2023-10-16 | 2024-03-22 | 河北双牛建材纤维素有限公司 | Method for preparing high-purity hydroxypropyl methyl cellulose |
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| CP03 | Change of name, title or address | ||
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Address after: 313000 No. 88, Zhongde Road, Linghu Town, Nanxun District, Huzhou City, Zhejiang Province (self declaration) Patentee after: Meixinjia Zhongwei Pharmaceutical Co.,Ltd. Address before: 313000 No.366 Zijing Road, Huzhou Economic and Technological Development Zone, Huzhou City, Zhejiang Province Patentee before: ZHEJIANG JOINWAY PHARMACEUTICAL CO.,LTD. |
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Denomination of invention: Green production method of hydroxypropyl methylcellulose Effective date of registration: 20220223 Granted publication date: 20191101 Pledgee: Huzhou Wuxing Rural Commercial Bank Co.,Ltd. Pledgor: Meixinjia Zhongwei Pharmaceutical Co.,Ltd. Registration number: Y2022980001769 |
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Address after: 313000 No. 366, Zijing Road, Longxi Street, South Taihu New District, Huzhou, Zhejiang Patentee after: Meixinjia Zhongwei Pharmaceutical Co.,Ltd. Address before: 313000 No. 88, Zhongde Road, Linghu Town, Nanxun District, Huzhou City, Zhejiang Province (self declaration) Patentee before: Meixinjia Zhongwei Pharmaceutical Co.,Ltd. |