CN101555285A - Preparation method of low-substituted hydroxypropyl cellulose - Google Patents
Preparation method of low-substituted hydroxypropyl cellulose Download PDFInfo
- Publication number
- CN101555285A CN101555285A CNA2008101636803A CN200810163680A CN101555285A CN 101555285 A CN101555285 A CN 101555285A CN A2008101636803 A CNA2008101636803 A CN A2008101636803A CN 200810163680 A CN200810163680 A CN 200810163680A CN 101555285 A CN101555285 A CN 101555285A
- Authority
- CN
- China
- Prior art keywords
- low
- substituted hydroxypropyl
- preparation
- reactor
- hydroxypropyl cellulose
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 229940031703 low substituted hydroxypropyl cellulose Drugs 0.000 title claims abstract description 22
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 claims abstract description 23
- -1 hydroxypropyl Chemical group 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000005406 washing Methods 0.000 claims abstract description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 73
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 27
- 229920000742 Cotton Polymers 0.000 claims description 21
- 229920002153 Hydroxypropyl cellulose Polymers 0.000 claims description 11
- 235000010977 hydroxypropyl cellulose Nutrition 0.000 claims description 11
- 239000000843 powder Substances 0.000 claims description 10
- 239000007921 spray Substances 0.000 claims description 8
- 238000010298 pulverizing process Methods 0.000 claims description 6
- 244000299507 Gossypium hirsutum Species 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 45
- 238000000034 method Methods 0.000 abstract description 15
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 abstract description 6
- 230000003301 hydrolyzing effect Effects 0.000 abstract description 2
- 235000013312 flour Nutrition 0.000 abstract 2
- 238000001035 drying Methods 0.000 abstract 1
- 230000002708 enhancing effect Effects 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 31
- 241000219146 Gossypium Species 0.000 description 20
- 239000003513 alkali Substances 0.000 description 18
- 238000006266 etherification reaction Methods 0.000 description 14
- 239000003814 drug Substances 0.000 description 8
- 238000007598 dipping method Methods 0.000 description 7
- 239000001863 hydroxypropyl cellulose Substances 0.000 description 7
- 230000035484 reaction time Effects 0.000 description 7
- 238000013019 agitation Methods 0.000 description 6
- 239000012670 alkaline solution Substances 0.000 description 6
- 229920002678 cellulose Polymers 0.000 description 6
- 239000001913 cellulose Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 239000000835 fiber Substances 0.000 description 6
- 230000007062 hydrolysis Effects 0.000 description 5
- 238000006460 hydrolysis reaction Methods 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- 235000013305 food Nutrition 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 238000007086 side reaction Methods 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- 229920002785 Croscarmellose sodium Polymers 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 1
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- VJHCJDRQFCCTHL-UHFFFAOYSA-N acetic acid 2,3,4,5,6-pentahydroxyhexanal Chemical compound CC(O)=O.OCC(O)C(O)C(O)C(O)C=O VJHCJDRQFCCTHL-UHFFFAOYSA-N 0.000 description 1
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 159000000007 calcium salts Chemical class 0.000 description 1
- 125000002057 carboxymethyl group Chemical group [H]OC(=O)C([H])([H])[*] 0.000 description 1
- 229940063834 carboxymethylcellulose sodium Drugs 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 235000021050 feed intake Nutrition 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 238000009702 powder compression Methods 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 238000005956 quaternization reaction Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000003232 water-soluble binding agent Substances 0.000 description 1
- 238000005550 wet granulation Methods 0.000 description 1
Landscapes
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention relates to a preparation method of low-substituted hydroxypropyl cellulose. The method comprises the following steps: A. adding flour to a reaction kettle; and B. adding soda solution and propylene oxide to the reaction kettle, and stirring; wherein, ratio of the flour, the soda, the propylene oxide and water is 1:0.4-1:0.3-0.5:0.4-3. The method further comprises steps of hydrolyzing, centrifuge washing, drying, crushing and mixing the obtained product in the reaction kettle. The method has the advantages of enhancing production efficiency, improving product quality and reducing production cost. The obtained low-substituted hydroxypropyl cellulose has stable hydroxypropyl content, and reaction yield is more than proportional yield.
Description
Technical field
The present invention relates to the preparation method of low-substituted hydroxypropyl cellulose, when in fields such as medicine, food, preparing preparation, with the slaking or the compressibility of this low-substituted hydroxypropyl cellulose adding so that medicine or food to be provided.
Background technology
Solid preparation in the field such as medicine, food, only the preparation by the main component preparation has following problem: when giving medicine, can not give full play to the effect of medicine because not obtaining enough slakings, and because its more weak compressibility makes the tablet of preparation thus or the shape of granule can not keep.In this case, the disintegrating agents such as calcium salt, cross-linked carboxymethyl cellulose sodium, cross-linked polyvinylpyrrolidone or carboxymethyl starch of low-substituted hydroxypropyl cellulose, Cellulose,ether with glycolic acid can improve its slaking by for example adding.In addition, can improve its compressibility by adding crystalline cellulose or water-soluble binder.Known low-substituted hydroxypropyl cellulose be a kind of uniqueness have slaking and compressible additive concurrently.
Because low-substituted hydroxypropyl cellulose is a non-ionic type, for example has advantage with the littler variation of ionic drug reaction causing.
The low additive that replaces light propyl cellulose useful as drug, in the prior art, the preparation were established of low-substituted hydroxypropyl cellulose is as follows: in the alkali lye system of certain proportioning, method with dipping makes purified cotton and caustic alkali carry out quaternization earlier, and then squeeze, alkali lye is separated with alkali fiber, alkali fiber and propylene oxide drop into squeezing in reactor after carry out etherification reaction, then by the etherification reaction material being hydrolyzed, neutralization, centrifuge washing, oven dry, operation such as pulverizing, confuse and obtain finished product.Concrete preparation method is after purified cotton is simply torn, immerse concentration and be in 10～25% the alkali lye, the dipping alkalization was squeezed the alkali fiber that obtains water capacity about 10～30% by squeezing machine after 3～4 hours, then alkali fiber is dropped in the reactor with the artificial way, in reactor, add propylene oxide, be warmed up to 70～90 ℃, carry out etherification reaction under the condition of the about 1.0Mpa of pressure, after reaction finishes, the etherification reaction thing is dropped into hydrolysis kettle, add aqueous hydrochloric acid, reaction is hydrolyzed, by centrifuge washing, dry then again, pulverize, operation such as confuse and obtain finished product.There is following shortcoming in this hydroxypropylcellulose preparation method: 1, alkalization, etherificate proceed step by step, repeat to feed intake, and labor strength is big, and production efficiency is low, feeds intake nearly 12 hours of a collection of total time spent; 2, alkalization is by dipping, squeezing, the alkalization lack of homogeneity, the alkali fiber water capacity instability of squeezing, follow-up etherification reaction is difficult to control, the corresponding instability of product yield and quality, for example the fluctuation of key index propoxyl content is very big changes in 4～14% scope, and the content fluctuation directly causes product disintegrating property instability, influences use properties; 3, the alkali liquor recovery set of squeezing generation is big with difficulty, causes the waste of sheet alkali and the problem of increase environmental protection treatment pressure, increases production cost.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of low-substituted hydroxypropyl cellulose, it is enhanced productivity, improves quality product, reduces production costs.
Foregoing invention purpose of the present invention is achieved through the following technical solutions:
A kind of preparation method of low-substituted hydroxypropyl cellulose may further comprise the steps:
A. cotton powder is added in the reactor;
B. simultaneously caustic soda soln and propylene oxide are joined in the reactor, stir;
The ratio of described cotton powder, caustic soda, propylene oxide and water is 1: 0.25～1: 0.3～0.5: 0.4～3.
Low-substituted hydroxypropyl cellulose of the present invention is cellulosic hydroxypropyl etherificate thing, and it is soluble in cold water, is heated to 50 ℃ gel takes place.Dissolve in methyl alcohol, ethanol, Virahol and the propylene glycol, it can be used for the tackiness agent of wet granulation in the medicine, also can do the dry adhesives of direct powder compression.
Cotton powder of the present invention is a purified cotton through the preliminary result who pulverizes, and preferred 60～100 orders of its granularity if select for use than the cotton powder of volume particle size then influence the speed and the yield of reaction, cause side reaction to increase if cotton powder particles is too small.
The ratio of described cotton powder, caustic soda, propylene oxide and water preferred 1: 0.4～0.5: 0.3～0.4: 0.6～1.25.
The ratio of described cotton powder, caustic soda, propylene oxide and water preferred 1: 0.8～1: 0.3～0.5: 0.6～1.25.
The ratio of various reactants that the present invention is preferred, creatively will alkalize and etherificate carry out synchronously, eliminated the number of drawbacks of prior art, and it has been generally acknowledged that above-mentioned two steps can not merge, because it is prior art is thought that above-mentioned two steps are too high to the conversion unit requirement, and the hydrolysis of initial ring Ethylene Oxide easily.The present invention is because the preferred amount and the form of above-mentioned reactant solved above-mentioned technology prejudice.
Cotton powder of the present invention, caustic soda, propylene oxide and water add in the reactor simultaneously, in aforesaid reaction vessel, alkalize simultaneously, etherification reaction obtains the etherification reaction thing, compare with the proceed step by step of prior art, the present invention once feeds intake, labor strength is little, the production efficiency height, a collection of total time spent that feeds intake significantly reduces, and only needs about 8 hours; It has removed steps such as dipping, squeezing, and its alkalization homogeneity is strong, has got rid of the unsettled defective of alkali fiber water capacity of squeezing in the prior art, and product yield and quality are corresponding stable, product propoxyl stable content.
Alkalization of the present invention, etherificate are carried out in reactor simultaneously, and the temperature in the reactor is 30～90 ℃, and preferred 42～48 ℃, pressure≤0.2Mpa, preferred pressure≤0.1Mpa.Churning time is 1～3hr, preferred 1.5～2.5hr.
The present invention can finish main body of the present invention reaction under above-mentioned reaction conditions, its reaction conditions requires lowly to equipment, and the side reaction of reaction is few, the product yield height.
Method of the present invention also comprise with products therefrom in the reactor be hydrolyzed, centrifuge washing, oven dry, the step pulverizing, confuse.
Described hydrolysing step promptly adds acid and gets final product in reactor, described acid can be hydrochloric acid, nitric acid, acetate etc.
Caustic soda soln of the present invention and propylene oxide can spray in the reactor by nozzle.
The present invention preferably stirs in reactor adding caustic soda soln and propylene oxide.
In sum, compared with prior art, the present invention has improved reaction process and the processing condition and the processing parameters such as reaction mass proportioning, reaction conditions of alkalization in the preparation low-substituted hydroxypropyl cellulose process, etherification reaction, has improved reaction efficiency, shorten reaction time, improved production efficiency; Improved the reaction homogeneity, product quality is improved; The present invention has increased the concentration of alkali lye, and it is very low to have changed in the prior art concentration of lye, be with the whole submergences of purified cotton, and the shortcoming that consumption is big, dipping time is long, the used concentration of lye of the method for the invention is higher, can guarantee that the alkali lye cumulative volume reduces.Therefore, the present invention has also reduced consumption, treatment capacity and the quantity discharged of alkali lye, reaches effects of energy saving and emission reduction simultaneously, has improved plant factor, has reduced labour intensity and production cost.
Embodiment
Embodiment one
Add entry 200kg, sodium hydroxide 50kg in agitation vat, stirring and dissolving is standby.
In reactor, add purified cotton 200kg (80 order), slowly (about 30 minutes) spray into alkaline solution and the propylene oxide 80kg for preparing then, ceaselessly stir, raw material alkalizes and etherification reaction simultaneously in reactor, temperature in the control reactor is at 42～48 ℃, reaction pressure 0.05MPa, reaction times 2.5hr.Obtain hydroxypropylcellulose finished product 195.6kg after finishing dealing with through hydrolysis, centrifuge washing, oven dry, pulverizing process after reaction finishes.Test by Chinese Pharmacopoeia 2005 editions, the propoxyl content of product, turgidity see Table 1, and wherein propoxyl content 8.8%.
Comparative example one
Is dipping back squeezing among the aqueous sodium hydroxide solution 2000kg of 15% (weight) with purified cotton 100kg at alkali concn, obtains soda cellulose 130kg.This soda cellulose 130kg joins in the reactor, in reactor, add propylene oxide 25kg while stirring 50 ℃ of reactions 1 hour, 60 ℃ of reactions 1 hour with 70 ℃ of reactions 2 hours, obtain resultant of reaction 140kg.Obtain product 90.2kg after finishing dealing with by hydrolysis, centrifuge washing, oven dry, pulverizing process again.By measure every performance index of its products obtained therefrom according to embodiment 1 described method, must the results are shown in Table 1 then.
Comparative example two
Is dipping back squeezing among the aqueous sodium hydroxide solution 2000kg of 20% (weight) with purified cotton 100kg at alkali concn, obtains soda cellulose 137kg.This soda cellulose 137kg joins in the reactor, in reactor, add propylene oxide 31kg while stirring 50 ℃ of reactions 1 hour, 60 ℃ of reactions 1 hour with 70 ℃ of reactions 2 hours, obtain resultant of reaction 135kg.Obtain product 91.4kg after finishing dealing with by hydrolysis, centrifuge washing, oven dry, pulverizing process again.By measure every performance index of its products obtained therefrom according to embodiment 1 described method, must the results are shown in Table 1 then.
Embodiment two
Add entry 250kg, sodium hydroxide 100kg in agitation vat, stirring and dissolving is standby.
In reactor, add purified cotton 200kg (60 order), slowly spray into the alkaline solution and the propylene oxide 100kg that prepare then, alkalize and etherification reaction 55～60 ℃ of temperature of reaction, reaction pressure 0.1MPa, reaction times 3hr simultaneously.Obtain hydroxypropylcellulose finished product 197.3kg after finishing dealing with through subsequent handling after reaction finishes.Through checking with quadrat method, quality product obviously is better than prior art products, and wherein propoxyl content 9.1%.
Embodiment three
Add entry 180kg, sodium hydroxide 75kg in agitation vat, stirring and dissolving is standby.
In reactor, add purified cotton 200kg (100 order), slowly spray into the alkaline solution and the propylene oxide 90kg that prepare then, alkalize and etherification reaction 81～88 ℃ of temperature of reaction, reaction pressure 0.15MPa, reaction times 1.5hr simultaneously.Obtain hydroxypropylcellulose finished product 194.5kg after finishing dealing with through subsequent handling after reaction finishes.Through checking with quadrat method, quality product obviously is better than prior art products, and wherein propoxyl content 8.9%.
Embodiment four
Add entry 80kg, sodium hydroxide 80kg in agitation vat, stirring and dissolving is standby.
In reactor, add purified cotton 200kg (80 order), slowly spray into the alkaline solution and the propylene oxide 60kg that prepare then, alkalize and etherification reaction 30～40 ℃ of temperature of reaction, reaction pressure 0.1MPa, reaction times 3hr simultaneously.Obtain hydroxypropylcellulose finished product 191.3kg after finishing dealing with through subsequent handling after reaction finishes.Through checking with quadrat method, quality product obviously is better than prior art products, and wherein propoxyl content 8.8%.
Embodiment five
Add entry 600kg, sodium hydroxide 80kg in agitation vat, stirring and dissolving is standby.
In reactor, add purified cotton 200kg (90 order), slowly spray into the alkaline solution and the propylene oxide 60kg that prepare then, alkalize and etherification reaction 60～70 ℃ of temperature of reaction, reaction pressure 0.2MPa, reaction times 3hr simultaneously.Obtain hydroxypropylcellulose finished product 190.3kg after finishing dealing with through subsequent handling after reaction finishes.Through checking with quadrat method, quality product obviously is better than prior art products, and wherein propoxyl content 8.9%.
Embodiment six
Add entry 160kg, sodium hydroxide 200kg in agitation vat, stirring and dissolving is standby.
In reactor, add purified cotton 200kg (60 order), slowly spray into the alkaline solution and the propylene oxide 60kg that prepare then, alkalize and etherification reaction 50～60 ℃ of temperature of reaction, reaction pressure 0.1MPa, reaction times 2.5hr simultaneously.Obtain hydroxypropylcellulose finished product 190.1kg after finishing dealing with through subsequent handling after reaction finishes.Through checking with quadrat method, quality product obviously is better than prior art products, and wherein propoxyl content 8.9%.
Table 1
| Title | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | Comparative Examples 1 | Comparative Examples 2 |
| Purified cotton is dropped into number | 200 | 200 | 200 | 200 | 200 | 200 | 100 | 100 |
| Output | 195.6 | 197.3 | 194.5 | 191.3kg | 190.3kg | 190.1kg | 90.2 | 91.4 |
| Yield | 97.8％ | 98.65％ | 97.25％ | 95.65％ | 95.15％ | 95.05％ | 90.2％ | 91.4％ |
| Propoxyl content | 8.8％ | 9.1％ | 8.9％ | 8.8％ | 8.9％ | 8.9％ | 4.2％ | 5.7％ |
| Turgidity ml | 21 | 22 | 21 | 22 | 20 | 20 | 8 | 11 |
Experimental result shows, adopts the propoxyl content of low-substituted hydroxypropyl cellulose of the method for the invention gained highly stable, and reaction yield is greater than the yield of Comparative Examples, and simultaneously as can be seen, its turgidity also obviously is better than Comparative Examples.
In addition, the W-response time of the present invention significantly reduces, and it is artificial, time cost has obtained effective reduction, and its alkali consumption also reduces greatly.
Claims (10)
1, a kind of preparation method of low-substituted hydroxypropyl cellulose may further comprise the steps:
A. cotton powder is added in the reactor;
B. simultaneously caustic soda soln and propylene oxide are joined in the reactor, stir;
The ratio of described cotton powder, caustic soda, propylene oxide and water is 1: 0.4～1: 0.3～0.5: 0.4～3.
2, the preparation method of low-substituted hydroxypropyl cellulose according to claim 1 is characterized in that: the temperature in the reactor is 30～90 ℃, pressure≤0.2Mpa.
3, the preparation method of low-substituted hydroxypropyl cellulose according to claim 1 is characterized in that: churning time is 1～3hr.
4, the preparation method of low-substituted hydroxypropyl cellulose according to claim 1 is characterized in that: it also comprise with products therefrom in the reactor be hydrolyzed, centrifuge washing, oven dry, the step pulverizing, confuse.
5, according to the preparation method of claim 1 or 2 or 3 or 4 described low-substituted hydroxypropyl celluloses, it is characterized in that: described caustic soda soln and propylene oxide spray in the reactor by nozzle.
6, the preparation method of low-substituted hydroxypropyl cellulose according to claim 2 is characterized in that: the temperature in the described reactor is 42～48 ℃.
7, the preparation method of low-substituted hydroxypropyl cellulose according to claim 3 is characterized in that: described churning time is 1.5～2.5hr.
8, according to the preparation method of claim 1 or 2 or 3 or 4 described low-substituted hydroxypropyl celluloses, it is characterized in that: the propoxyl content 8.8～9.1% of the low-substituted hydroxypropyl cellulose of gained.
9, according to the preparation method of claim 1 or 2 or 3 or 4 described low-substituted hydroxypropyl celluloses, it is characterized in that: the pressure≤0.1Mpa in the described reactor.
10, according to the preparation method of claim 1 or 2 or 3 or 4 described low-substituted hydroxypropyl celluloses, it is characterized in that: stir in reactor adding caustic soda soln and propylene oxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008101636803A CN101555285B (en) | 2008-12-19 | 2008-12-19 | Preparation method of low-substituted hydroxypropyl cellulose |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008101636803A CN101555285B (en) | 2008-12-19 | 2008-12-19 | Preparation method of low-substituted hydroxypropyl cellulose |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101555285A true CN101555285A (en) | 2009-10-14 |
| CN101555285B CN101555285B (en) | 2010-12-01 |
Family
ID=41173582
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2008101636803A Active CN101555285B (en) | 2008-12-19 | 2008-12-19 | Preparation method of low-substituted hydroxypropyl cellulose |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101555285B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102924609A (en) * | 2012-12-04 | 2013-02-13 | 新疆光大山河化工科技有限公司 | Method for producing low-substituted hydroxypropyl cellulose via fractional step method |
| CN109369810A (en) * | 2018-09-18 | 2019-02-22 | 中国制浆造纸研究院有限公司 | Carbamoylethyl fento cellulose and preparation method thereof |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4044689B2 (en) * | 1998-12-07 | 2008-02-06 | 信越化学工業株式会社 | Method for producing low substituted hydroxypropylcellulose |
| JP3572213B2 (en) * | 1999-01-18 | 2004-09-29 | 信越化学工業株式会社 | Low substituted hydroxypropylcellulose |
| EP1054019A1 (en) * | 1999-05-18 | 2000-11-22 | Shin-Etsu Chemical Co., Ltd. | Low-substituted hydroxypropyl cellulose |
| US6680069B1 (en) * | 1999-11-09 | 2004-01-20 | Shin-Etsu Chemical Co., Ltd. | Low-substituted hydroxypropyl cellulose and process for manufacturing the same |
| JP3552160B2 (en) * | 2000-01-14 | 2004-08-11 | 信越化学工業株式会社 | Method for forming low-substituted hydroxypropylcellulose particles |
-
2008
- 2008-12-19 CN CN2008101636803A patent/CN101555285B/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102924609A (en) * | 2012-12-04 | 2013-02-13 | 新疆光大山河化工科技有限公司 | Method for producing low-substituted hydroxypropyl cellulose via fractional step method |
| CN109369810A (en) * | 2018-09-18 | 2019-02-22 | 中国制浆造纸研究院有限公司 | Carbamoylethyl fento cellulose and preparation method thereof |
| CN109369810B (en) * | 2018-09-18 | 2021-06-15 | 中国制浆造纸研究院有限公司 | Carbamoylethyl microfibrillated cellulose and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101555285B (en) | 2010-12-01 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101260158A (en) | Method for preparing hydroxypropylmethylcellulose | |
| CN100455601C (en) | Modification method of cellulose ether product | |
| CN103910803B (en) | Method for preparing cellulose ether having low degree of polymerization and cellulose ether prepared thereby | |
| CN104592400B (en) | A kind of preparation method of microcrystalline Cellulose | |
| JPH0476361B2 (en) | ||
| CN102477100A (en) | Esterification-etherification dual-modified starch and solid phase preparation method thereof | |
| WO2022007454A1 (en) | Modified hydroxypropyl methyl cellulose for enhanced ceramic tile adhesive, and preparation method therefor and use thereof | |
| CN101001881A (en) | Process for producing cellulose derivative with improved solubility | |
| CN101585883A (en) | High-purity sodium carboxymethyl starch, preparation method thereof and application thereof | |
| CN105295063A (en) | Surface-modified microcrystalline cellulose and preparation method thereof | |
| CN101555285B (en) | Preparation method of low-substituted hydroxypropyl cellulose | |
| CN103242453A (en) | Method for preparing low-viscosity sodium carboxymethylcellulose | |
| CN108191993B (en) | A kind of sodium alginate and its preparation method and application | |
| CN104311682A (en) | Preparation method of medicinal carboxymethyl starch | |
| CN101423588A (en) | Industrial synthesis method for producing high water absorption resin | |
| CN102276733B (en) | Method for preparing ethyl cellulose with high degree of substitution | |
| CN106750439A (en) | A kind of utilization bagasse prepares the method and obtained packaging film of packaging film | |
| CN1123575C (en) | Process for preparing hydroxypropylmethyl cellulose by one-step method | |
| CN106432515A (en) | Preparation method of high substitution degree carboxymethyl cellulose sodium and application thereof | |
| CN104892773A (en) | Preparation method of high-substitution-degree sodium carboxymethylcellulose | |
| CN105111317A (en) | Preparation method of cellulose ether and cellulose ether obtained in same | |
| CN101830991A (en) | Rapid production technology for carboxymethyl cellulose by aqueous medium process | |
| CN109970873B (en) | Preparation method of pharmaceutical adjuvant grade microcrystalline cellulose | |
| CN104098703A (en) | Preparation method of CMC (carboxymethyl cellulose) | |
| CN107353434A (en) | A kind of preparation method using hydroxypropylation lobster shell as primary raw material composite water conservation material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C56 | Change in the name or address of the patentee | ||
| CP03 | Change of name, title or address |
Address after: 313000, No. 366, Bauhinia Road, Huzhou economic and Technological Development Zone, Zhejiang, Huzhou Patentee after: ZHEJIANG JOINWAY PHARMACEUTICAL CO.,LTD. Address before: 313000, No. 366, Bauhinia Road, Huzhou Economic Development Zone, Zhejiang, Huzhou Patentee before: ZHEJIANG JOINWAY PHARMACEUTICAL Co.,Ltd. |
|
| CP03 | Change of name, title or address | ||
| CP03 | Change of name, title or address |
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. |
|
| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: Preparation method of low substituted hydroxypropyl cellulose Effective date of registration: 20220223 Granted publication date: 20101201 Pledgee: Huzhou Wuxing Rural Commercial Bank Co.,Ltd. Pledgor: Meixinjia Zhongwei Pharmaceutical Co.,Ltd. Registration number: Y2022980001769 |
|
| CP02 | Change in the address of a patent holder | ||
| CP02 | Change in the address of a patent holder |
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. |