CN1005193B - Preparation technology of cyanoethyl cellulose - Google Patents
Preparation technology of cyanoethyl cellulose Download PDFInfo
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- CN1005193B CN1005193B CN86108562.0A CN86108562A CN1005193B CN 1005193 B CN1005193 B CN 1005193B CN 86108562 A CN86108562 A CN 86108562A CN 1005193 B CN1005193 B CN 1005193B
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- cellulose
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- dipping
- sodium hydroxide
- cyanoethyl
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Abstract
The present invention belongs to technology for preparing cyanoethyl cellulose acetate which is a derivative of cellulose mixed ester, which comprises the steps: cellulose is immersed and activated twice by sodium hydroxide; the cyanoethylation reaction is carried out at negative pressure, and the acetylation reaction is carried out in the existence of a catalyst. The present invention has the characteristics that the product with the given ratio of ester radicals can be prepared, the medicine consumption is low, and the reaction time is short. Various membranes which are prepared by cyanoethyl cellulose acetate prepared by the technology of the present invention have the advantages of high water flux, high catching rate, favorable microbe resistant performance and favorable chemical stability.
Description
The invention relates to the preparation technology of derivatived cellulose mould material-cyanoethyl cellulose (mixed ester ether derivant).Reverse osmosis technology is a kind of new technology that early sixties grows up.At present become important separation method and be widely used in seawater and brackish water desalination.The purification of industrial pollution water, food, medicine and other industrial separation are concentrated etc.Though the Cellulose diacetate film is in industrial application, because shortcomings such as not anti-microbial attack and poor chemical stability, thereby range of application is subjected to certain limitation.Some shortcoming at Cellulose diacetate.The present invention discovers substituent synergistic effect, adopts twice dipping of aqueous sodium hydroxide solution activated cellulose.Under negative pressure, carry out cyanoethylation reaction and in the presence of catalyzer, carry out acetylizad novel process.The cyanoethyl cellulose that has prepared various different ratios cyanoethyl substitution values and degree of substitution with acetyl group.The molten Jie performance of this product in acetone and other organic solvent is good, is processed into various separatory membranes easily, relatively has high water flux with existing Cellulose diacetate film.High rejection.Excellent anti-microbial performance and better chemical stability.This processing method compares with method of the prior art (USSR590312.612933), and its process characteristic is that the reaction times is short, and drug dosage is few, can prepare the cyanoethyl cellulose of different degree of substitution under different reaction conditionss.The cyanoethyl substitution value of product is 0.26～0.77, and ethanoyl is 2.0～2.7.
The embodiment of this processing method is as follows:
With linter pulp is that 14～20% liquor ratios are 1: 20 sodium hydroxide solution dipping one hour with concentration at room temperature, presses and removes unnecessary sodium hydroxide solution, floods 20～30 minutes with being lower than 5% alkaline solution again.Pressure is removed unnecessary alkali lye, makes it reach the fine composition of needed alkali.After this soda cellulose is placed encloses container to add the vinyl cyanide of Mierocrystalline cellulose 5～30% under negative pressure, under agitation control reaction temperature is 23～35 ℃, reacts after 20～40 minutes, with the diluted acid neutralization, is washed till neutrality, drying.
With the above-mentioned cyanoethyl cellulose that makes; adding aceticanhydride, acetic acid carries out acetylize, esterification under sulfuric acid catalysis temperature is 35 ℃; reacted 3～4 hours; water was situated between 3～5 hours; water Jie temperature is 50～55 ℃; Mierocrystalline cellulose: acetic acid+aceticanhydride: sulfuric acid=1: 8～9: 0.1, under the differential responses condition, can prepare the cyanoethyl cellulose of different degree of substitution.
Embodiment one
Linter pulp was dipped in the sodium hydroxide solution (concentration is 14%) dipping one hour.Liquefaction is 1: 20, pressure goes unnecessary alkali lye to flood 20 minutes with 5% sodium hydroxide solution again, pressure is removed unnecessary alkali lye, then soda cellulose is placed encloses container to add vinyl cyanide 20%(to cellulose amount) reacted 40 minutes down in 30 ℃, add in the diluted acid extremely neutral with washing, drying adds acetic acid, aceticanhydride, under sulfuric acid catalysis, carry out esterification, water is situated between, Mierocrystalline cellulose: acetic acid+aceticanhydride: sulfuric acid=1: 8.5: 0.1,35 ℃ of esterification temperatures reacted 3～5 hours, water Jie temperature is 50～55 ℃, water was situated between 3～5 hours, and behind the esterification catalysis, the washing of precipitate drying makes the cyanoethyl cellulose product.Product index is that the cyanoethyl substitution value is 0.37, and degree of substitution with acetyl group is 2.25.
Embodiment two
Linter pulp was dipped in 18 sodium hydroxide solutions one hour, and liquor ratio is 1: 20, presses and removes unnecessary alkali lye, soaks 20 minutes with 4.5% sodium hydroxide solution again, presses and removes unnecessary alkali lye, makes it meet the requirements of the soda cellulose composition.The vinyl cyanide that in encloses container, adds cellulose amount 30% then; neutralize with acid after 30 minutes 35 ℃ of reactions; the esterification process esterification among the embodiment one is pressed in the dry back of washing; water Jie washing of precipitate after drying obtains the cyanoethyl cellulose product; product index is a cyanoethyl substitution value 0.77, degree of substitution with acetyl group 2.14.
Claims (9)
1, a kind of preparation technology of derivatived cellulose mould material-cyanoethyl cellulose, it comprises with alkaline solution dipping linter pulp and cyanoethylation under certain condition, and carries out esterification in the presence of catalyzer, its preparation technology's feature is as follows:
(1) linter pulp was with 14%～20% sodium hydroxide solution dipping one hour, and liquefaction is 1: 20, after the squeezing again the sodium hydroxide solution with 4.5～5% flooded 20～30 minutes, make soda cellulose,
(2) under negative pressure the soda cellulose of above-mentioned preparation and the vinyl cyanide that is equivalent to cellulose amount 5～30% are reacted, neutralizing with acid then is washed till neutrality, makes cyanoethyl cellulose,
(3) cyanoethyl cellulose for preparing is carried out acetylize with acetic acid, aceticanhydride under sulfuric acid catalysis.3～4 hours reaction times.
2, according to described in the claim 1 to it is characterized by dipping temperature with sodium hydroxide dipping be 20～30 ℃.
3, according to it is characterized by the dipping back with sodium hydroxide dipping and press and go unnecessary alkali lye to make it reach needed soda cellulose to form described in the claim 1.
4, according to the reaction of described Mierocrystalline cellulose of claim 1 and vinyl cyanide, it is characterized by temperature of reaction is 23～35 ℃.
5, according to the reaction of Mierocrystalline cellulose described in the claim 1 and vinyl cyanide, it is characterized by the reaction times is 20～40 minutes.
6, according to the esterification described in the claim 1, the material ratio that it is characterized by reaction is a Mierocrystalline cellulose: aceticanhydride+acetic acid: sulfuric acid=1: 8～9: 0.1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN86108562.0A CN1005193B (en) | 1986-12-15 | 1986-12-15 | Preparation technology of cyanoethyl cellulose |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN86108562.0A CN1005193B (en) | 1986-12-15 | 1986-12-15 | Preparation technology of cyanoethyl cellulose |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN86108562A CN86108562A (en) | 1988-06-29 |
| CN1005193B true CN1005193B (en) | 1989-09-20 |
Family
ID=4803975
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN86108562.0A Expired CN1005193B (en) | 1986-12-15 | 1986-12-15 | Preparation technology of cyanoethyl cellulose |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1005193B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8729185B2 (en) * | 2011-04-05 | 2014-05-20 | Shin-Etsu Chemical Co., Ltd. | Method for producing 2-cyanoethyl group-containing organic compound |
| CN106866826A (en) * | 2017-04-05 | 2017-06-20 | 深圳市佩成科技有限责任公司 | The preparation method of cyanethyl cellulose derivative |
| CN113299981B (en) * | 2020-02-21 | 2022-12-06 | 广州天赐高新材料股份有限公司 | Solid polymer electrolyte membrane, preparation method and application thereof |
-
1986
- 1986-12-15 CN CN86108562.0A patent/CN1005193B/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| CN86108562A (en) | 1988-06-29 |
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