SU612933A1 - Method of obtaining aceto-mixed cellulose esters - Google Patents
Method of obtaining aceto-mixed cellulose estersInfo
- Publication number
- SU612933A1 SU612933A1 SU762414030A SU2414030A SU612933A1 SU 612933 A1 SU612933 A1 SU 612933A1 SU 762414030 A SU762414030 A SU 762414030A SU 2414030 A SU2414030 A SU 2414030A SU 612933 A1 SU612933 A1 SU 612933A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- aceto
- obtaining
- cellulose esters
- mixed cellulose
- cellulose
- Prior art date
Links
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- Polysaccharides And Polysaccharide Derivatives (AREA)
Description
1one
Изобретение относитс к области получени производных целлюлозы, а именно к синтезу ацетосмешанных эфиров целлюлозы, которые могут быть использованы в качестве антистатиков , загустителей, ионообменников, нолимеров медицинского назначени .The invention relates to the field of producing cellulose derivatives, namely, to the synthesis of cellulose aceto-mixed cellulose ethers, which can be used as antistatic agents, thickeners, ion exchangers, medical grade polymers.
Известен двухстадийный способ получени ацетосмешанных эфиров путем введени в молекулу целлюлозы сначала одного типа грунп и выделени полученного продукта, затем последующего превращени его вторым этерифицирующим агентом 1.A two-stage process for the preparation of acetal mixed ethers is known by first introducing one type of primer into the cellulose molecule and isolating the product obtained, then transforming it with a second esterifying agent 1.
Способ состоит в следующем. На первой стадии хлопковый линте2 активируют 2,5 ч 10-кратным количеством 18%-ной щелочи NaOH при 0°С, после чего отжимают до 3- 4-кратного веса. Акрилонитрил подают в количестве 20 моль на 1 моль ангидроглюкозного звена. Синтез провод т при 18-20°С в течение 2-48 ч при интенсивном размещивании . Реакционную массу нейтрализуют 5%-ной лед ной уксусной кислотой в спирте до нейтральной реакции. Эфир многократно промывают дистиллированной водой, переосаждают из раствора в диметилформамиде и экстрагируют спиртом 12-16 ч. После чего высушивают в вакуум-сушке при 40°С.The method consists in the following. In the first stage, cotton lint2 is activated for 2.5 hours with a 10-fold amount of 18% alkali NaOH at 0 ° C, after which it is squeezed to 3- 4-fold weight. Acrylonitrile is fed in an amount of 20 mol per 1 mol of the anhydroglucose unit. The synthesis is carried out at 18-20 ° C for 2-48 hours with intensive placement. The reaction mass is neutralized with 5% glacial acetic acid in alcohol until neutral. The ether is repeatedly washed with distilled water, replanted from the solution in dimethylformamide and extracted with alcohol for 12-16 hours. After that, they are dried in a vacuum drying at 40 ° C.
На второй стадии способа навеску полученной цианэтилцеллюлозы-10 г (YCH2CH2CN 158), этерифицируют при 30°С в течениеIn the second stage of the process, the weight of the obtained cyanoethyl cellulose 10 g (YCH2CH2CN 158) is etherified at 30 ° C for
3,5 ч ацетилирующей смесью 10,2 моль уксусного ангидрида, 19,3 моль четыреххлористого углерода и 2,1 моль хлорной кислоты. Продукт нейтрализуют 5%-ным раствором3.5 h with an acetylating mixture of 10.2 mol of acetic anhydride, 19.3 mol of carbon tetrachloride and 2.1 mol of perchloric acid. The product is neutralized with a 5% solution.
NaHCOs, отмывают дистиллированной водой, спиртом и эфиром.NaHCOs, washed with distilled water, alcohol and ether.
Однако в процессе по известному способу расходуютс большие количества реактивов и воды, способ вл етс громоздким из-за трудоемкой операции выделени продукта первой этерификации - простого эфира, отмывки его и сушки.However, in the process according to a known method, large quantities of reagents and water are consumed, the method is cumbersome due to the time-consuming operation of isolating the first esterification product — an ether, washing it and drying it.
Цель изобретени - упрощение способа получени ацетосмешанных эфиров, одностадийное получение растворимых в органических и неорганических растворител х ацетосмешанных эфиров целлюлозы, содержащих нар ду с ацетильными простые эфирные группы.The purpose of the invention is to simplify the process for the preparation of acetal mixed ethers, one-step preparation of acetal mixed cellulose ethers, which, in addition to acetyl ethers, are soluble in organic and inorganic solvents.
Дл этого по предлагаемому способу целлюлозу обрабатывают водным раствором едкого натра, этерифицируют акрилонитрилом (АН) или монохлоруксусной кислотой (МХК) дл введени простых эфирных группFor this, according to the proposed method, the cellulose is treated with an aqueous solution of caustic soda, esterified with acrylonitrile (AH) or monochloroacetic acid (MHC) for the introduction of ether groups
(/п 1:0,5-2,0), затем добавл ют уксусный ангидрид и серную кислоту в качестве катализатора (т 1:14,0-15,5), ацетилиру полученный продукт до образовани однородного гомогенного сиропа, который высаживают(/ p 1: 0.5-2.0), then acetic anhydride and sulfuric acid as a catalyst (m 1: 14.0-15.5) are added, the product obtained is acetylated to form a homogeneous homogeneous syrup, which is planted
и промывают.and washed.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SU762414030A SU612933A1 (en) | 1976-08-02 | 1976-08-02 | Method of obtaining aceto-mixed cellulose esters |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SU762414030A SU612933A1 (en) | 1976-08-02 | 1976-08-02 | Method of obtaining aceto-mixed cellulose esters |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| SU612933A1 true SU612933A1 (en) | 1978-06-30 |
Family
ID=20680564
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| SU762414030A SU612933A1 (en) | 1976-08-02 | 1976-08-02 | Method of obtaining aceto-mixed cellulose esters |
Country Status (1)
| Country | Link |
|---|---|
| SU (1) | SU612933A1 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5668273A (en) * | 1996-01-29 | 1997-09-16 | Eastman Chemical Company | Carboxyalkyl cellulose esters |
| US7026470B2 (en) | 2000-11-01 | 2006-04-11 | Eastman Chemical Corporation | Use of carboxymethyl cellulose acetate butyrate as a precoat or size for cellulosic man-made fiber boards |
-
1976
- 1976-08-02 SU SU762414030A patent/SU612933A1/en active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5668273A (en) * | 1996-01-29 | 1997-09-16 | Eastman Chemical Company | Carboxyalkyl cellulose esters |
| US7026470B2 (en) | 2000-11-01 | 2006-04-11 | Eastman Chemical Corporation | Use of carboxymethyl cellulose acetate butyrate as a precoat or size for cellulosic man-made fiber boards |
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