CN103214590B - A kind of preparation method of cyanoethyl starch - Google Patents
A kind of preparation method of cyanoethyl starch Download PDFInfo
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- CN103214590B CN103214590B CN201310173638.0A CN201310173638A CN103214590B CN 103214590 B CN103214590 B CN 103214590B CN 201310173638 A CN201310173638 A CN 201310173638A CN 103214590 B CN103214590 B CN 103214590B
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- CN
- China
- Prior art keywords
- starch
- cyanoethyl
- cyanoethyl starch
- parts
- crude product
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- 229920002472 Starch Polymers 0.000 title claims abstract description 98
- 239000008107 starch Substances 0.000 title claims abstract description 98
- 235000019698 starch Nutrition 0.000 title claims abstract description 98
- 125000001731 2-cyanoethyl group Chemical group [H]C([H])(*)C([H])([H])C#N 0.000 title claims abstract description 75
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 18
- 238000007670 refining Methods 0.000 claims abstract description 15
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 claims abstract description 7
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims abstract description 7
- 229910052938 sodium sulfate Inorganic materials 0.000 claims abstract description 7
- 235000011152 sodium sulphate Nutrition 0.000 claims abstract description 7
- 239000008187 granular material Substances 0.000 claims abstract description 6
- 230000008961 swelling Effects 0.000 claims abstract description 6
- 244000017020 Ipomoea batatas Species 0.000 claims abstract description 5
- 235000002678 Ipomoea batatas Nutrition 0.000 claims abstract description 5
- 239000003112 inhibitor Substances 0.000 claims abstract description 5
- 229920001592 potato starch Polymers 0.000 claims abstract description 5
- 239000012043 crude product Substances 0.000 claims description 22
- 239000011259 mixed solution Substances 0.000 claims description 20
- 238000005119 centrifugation Methods 0.000 claims description 14
- 239000000047 product Substances 0.000 claims description 11
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 10
- 235000013336 milk Nutrition 0.000 claims description 10
- 239000008267 milk Substances 0.000 claims description 10
- 210000004080 milk Anatomy 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 7
- 238000006266 etherification reaction Methods 0.000 claims description 6
- 229960000583 acetic acid Drugs 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 239000004744 fabric Substances 0.000 claims description 5
- 239000000706 filtrate Substances 0.000 claims description 5
- 239000012362 glacial acetic acid Substances 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 230000020477 pH reduction Effects 0.000 claims description 5
- 238000000746 purification Methods 0.000 claims description 5
- 238000005516 engineering process Methods 0.000 abstract description 5
- 238000000034 method Methods 0.000 abstract description 4
- 239000011230 binding agent Substances 0.000 abstract description 2
- 239000003795 chemical substances by application Substances 0.000 abstract description 2
- 230000001681 protective effect Effects 0.000 abstract 2
- 239000011248 coating agent Substances 0.000 abstract 1
- 238000000576 coating method Methods 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 239000012528 membrane Substances 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 238000000926 separation method Methods 0.000 abstract 1
- 239000002002 slurry Substances 0.000 abstract 1
- 239000004753 textile Substances 0.000 abstract 1
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 4
- 240000003183 Manihot esculenta Species 0.000 description 2
- 235000016735 Manihot esculenta subsp esculenta Nutrition 0.000 description 2
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 235000013312 flour Nutrition 0.000 description 2
- 238000005457 optimization Methods 0.000 description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 description 2
- 238000009941 weaving Methods 0.000 description 2
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000001046 anti-mould Effects 0.000 description 1
- -1 cyanoethyl starch Chemical compound 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000001632 sodium acetate Substances 0.000 description 1
- 229960004249 sodium acetate Drugs 0.000 description 1
- 235000017281 sodium acetate Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Landscapes
- Grain Derivatives (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The present invention relates to a kind of preparation method of cyanoethyl starch.Cyanoethyl starch can be used as the binding agent of slurry and coating.This cyanoethyl starch can remain on textiles and paper tightly, form the protective film that intensity is higher, and this layer of protective membrane has mildew-proof function.Described preparation method take vinyl cyanide as etherifying agent, and preferred sweet potato starch is raw material, and sodium sulfate is starch granules swelling inhibitor, and sodium hydroxide is catalyzer, reacts in aqueous.The production stage of present method comprises mixing, alkalization, etherificate, separation, acidifying, refining, dry.Utilize this preparation method can prepare satisfactory cyanoethyl starch, and preparation technology is simple, controllability is strong.
Description
Technical field
The present invention relates to a kind of preparation method of cyanoethyl starch.
Background technology
Cyanoethyl starch has purposes comparatively widely.Can be used as the industries such as weaving, papermaking and binding agent.It is that it has the ability of anti-bacteria and mould that cyanoethyl starch also has an important feature, and be therefore used in the industry such as papermaking and weaving, product has the feature of mildew-resistant.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of preparation method of cyanoethyl starch, utilizes this preparation method can prepare satisfactory cyanoethyl starch, and preparation technology is simple, controllability is strong.
For solving the problems of the technologies described above, the invention provides a kind of preparation method of cyanoethyl starch, comprising the following steps:
(1) mix: under whipped state, 100 parts of starch being joined 500-600 parts, to be dissolved with mass percent concentration be in the aqueous solution of 18-25% starch granules swelling agent, and temperature controls at 35-45 DEG C, do not stop to stir, obtain starch milk;
(2) alkalize: under whipped state, add 0.8-1.1 parts of catalyzer in starch milk, temperature controls at 35-45 DEG C, and alkalization time is 40-50min, obtains mixed solution;
(3) etherificate: under whipped state, keep temperature to be 35-45 DEG C, add 3.1-3.5 parts of vinyl cyanide in mixed solution, react 3.5-4h under 35-45 DEG C of conditions after, etherification reaction terminates, and obtains cyanoethyl starch mixed solution;
(4) be separated: cyanoethyl starch mixed solution is proceeded in the whizzer of band filter cloth and be separated to obtain the first cyanoethyl starch crude product;
(5) acidifying: under whipped state, the first cyanoethyl starch crude product being dissolved in 220-300 parts of mass percent concentrations is in the aqueous ethanolic solution of 81%, add 2.5-2.8 parts of Glacial acetic acid, react 45-50min under 40-45 DEG C of conditions after, acidification reaction terminates, and obtains the second cyanoethyl starch crude product after centrifugation;
(6) refining: the second cyanoethyl starch crude product to be washed, centrifugation, obtain refining cyanoethyl starch wet product;
(7) dry: namely to obtain cyanoethyl starch by after the drying of refining cyanoethyl starch wet product.
As optimization of the present invention, described starch is the one in sweet potato starch, W-Gum or tapioca (flour).
Described starch granules swelling inhibitor is sodium sulfate or sodium-chlor, and concentration is in aqueous 18-25%.
Described catalyzer is the one in sodium hydroxide, potassium hydroxide or sodium carbonate.
The step of described washing, centrifugation is: with the mass percent concentration that temperature is 20-40 DEG C be 81% aqueous ethanolic solution the second cyanoethyl starch crude product is washed, washing liquid level is as the criterion with submergence cyanoethyl starch, after stirring 20min, centrifugation obtains primary purification cyanoethyl starch; Repeat above-mentioned steps 2-3 times, when filtrate pH >=5.6.
Described drying is dry 2-3h in 80-85 DEG C of baking ovens.
As further optimization of the present invention, described starch is sweet potato starch.
Described starch granules swelling inhibitor is sodium sulfate.
Described catalyzer is sodium hydroxide.
For the purpose of concise explanation problem, below to the preparation method of a kind of cyanoethyl starch of the present invention all referred to as present method.
Starch having under catalyzer existent condition with the chemical equation of vinyl cyanide is:
St-OH+CH
2＝CH-CN→St-O-CH
2CH
2CN
In the method, strictly to control etherification reaction temperature, when temperature is higher than 45 DEG C, have following side reaction to occur:
St-O-CH
2CH
2CN+H
2O→St-O-CH
2CH
2CONH
2
St-O-CH
2CH
2CONH
2+NaOH→St-O-CH
2CH
2COONa+NH
3
In the method, refining object is the impurity such as sodium sulfate in removing cyanoethyl starch and sodium-acetate.
Utilize this preparation method can prepare satisfactory cyanoethyl starch, and preparation technology is simple, controllability is strong.
Embodiment
Below by specific embodiment, the invention will be further described:
Embodiment 1:
A preparation method for cyanoethyl starch, comprises the following steps:
(1) mix: under whipped state, 100 parts of sweet potato starchs being joined 550 parts, to be dissolved with mass percent concentration be in the aqueous solution of the sodium sulfate of 22%, and temperature controls at 35 DEG C, do not stop to stir, obtain starch milk;
(2) alkalize: under whipped state, add 1 part of sodium hydroxide in starch milk, temperature controls at 35 DEG C, and alkalization time is 45min, obtains mixed solution;
(3) etherificate: under whipped state, keep temperature to be 35 DEG C, in mixed solution, add 3.3 parts of vinyl cyanide, react 3.5h under 35 DEG C of conditions after, etherification reaction terminates, and obtains cyanoethyl starch mixed solution;
(4) be separated: cyanoethyl starch mixed solution is proceeded in the whizzer of band filter cloth and be separated to obtain the first cyanoethyl starch crude product;
(5) acidifying: under whipped state, the first cyanoethyl starch crude product being dissolved in 260 parts of mass percent concentrations is in the aqueous ethanolic solution of 81%, add 2.6 parts of Glacial acetic acid, react 45min under 40 DEG C of conditions after, acidification reaction terminates, and obtains the second cyanoethyl starch crude product after centrifugation;
(6) refining: to the second cyanoethyl starch crude product temperature be 20 DEG C, mass percent concentration be 81% aqueous ethanolic solution wash, washing liquid level is as the criterion with submergence cyanoethyl starch, after stirring 20min, centrifugation obtains primary purification cyanoethyl starch; Repeat above-mentioned steps 2 times, filtrate pH >=5.6, obtain refining cyanoethyl starch wet product;
(7) dry: cyanoethyl starch wet product dry 2.5h in 80 DEG C of baking ovens will to be refined, obtain cyanoethyl starch.
Embodiment 2:
A preparation method for cyanoethyl starch, comprises the following steps:
(1) mix: under whipped state, 100 parts of W-Gums being joined 500 parts, to be dissolved with mass percent concentration be in the aqueous solution of 25% sodium-chlor, and temperature controls at 40 DEG C, do not stop to stir, obtain starch milk;
(2) alkalize: under whipped state, add 0.8 part of potassium hydroxide in starch milk, temperature controls at 40 DEG C, and alkalization time is 40min, obtains mixed solution;
(3) etherificate: under whipped state, keep temperature to be 40 DEG C, in mixed solution, add 3.1 parts of vinyl cyanide, react 3.5h under 40 DEG C of conditions after, etherification reaction terminates, and obtains cyanoethyl starch mixed solution;
(4) be separated: cyanoethyl starch mixed solution is proceeded in the whizzer of band filter cloth and be separated to obtain the first cyanoethyl starch crude product;
(5) acidifying: under whipped state, the first cyanoethyl starch crude product being dissolved in 220 parts of mass percent concentrations is in the aqueous ethanolic solution of 81%, add 2.5 parts of Glacial acetic acid, react 45min under 45 DEG C of conditions after, acidification reaction terminates, and obtains the second cyanoethyl starch crude product after centrifugation;
(6) refining: to the second cyanoethyl starch crude product temperature be 30 DEG C, mass percent concentration be 81% aqueous ethanolic solution wash, washing liquid level is as the criterion with submergence cyanoethyl starch, after stirring 20min, centrifugation obtains primary purification cyanoethyl starch; Repeat above-mentioned steps 2 times, filtrate pH >=5.6, obtain refining cyanoethyl starch wet product;
(7) dry: by refining cyanoethyl starch wet product dry 2h in 85 DEG C of baking ovens of preparation, to obtain cyanoethyl starch.
Embodiment 3:
A preparation method for cyanoethyl starch, comprises the following steps:
(1) mix: under whipped state, 100 portions of tapioca (flour)s being joined 600 parts, to be dissolved with mass percent concentration be in the aqueous solution of 18% sodium sulfate, and temperature controls at 45 DEG C, do not stop to stir, obtain starch milk;
(2) alkalize: under whipped state, add 1.1 parts of sodium carbonate in starch milk, temperature controls at 45 DEG C, and alkalization time is 50min, obtains mixed solution;
(3) etherificate: under whipped state, keep temperature to be 45 DEG C, in mixed solution, add 3.5 parts of vinyl cyanide, react 4h under 45 DEG C of conditions after, etherification reaction terminates, and obtains cyanoethyl starch mixed solution;
(4) be separated: cyanoethyl starch mixed solution is proceeded in the whizzer of band filter cloth and be separated to obtain the first cyanoethyl starch crude product;
(5) acidifying: under whipped state, the first cyanoethyl starch crude product being dissolved in 300 parts of mass percent concentrations is in the aqueous ethanolic solution of 81%, add 2.8 parts of Glacial acetic acid, react 50min under 45 DEG C of conditions after, acidification reaction terminates, and obtains the second cyanoethyl starch crude product after centrifugation;
(6) refining: to the second cyanoethyl starch crude product temperature be 40 DEG C, mass percent concentration be 81% aqueous ethanolic solution wash, washing liquid level is as the criterion with submergence cyanoethyl starch, after stirring 20min, centrifugation obtains primary purification cyanoethyl starch; Repeat above-mentioned steps 3 times, filtrate pH >=5.6, obtain refining cyanoethyl starch wet product;
(7) dry: by refining cyanoethyl starch wet product dry 3h in 85 DEG C of baking ovens of preparation, to obtain cyanoethyl starch.
Claims (1)
1. a preparation method for cyanoethyl starch, comprises the following steps:
(1) mix: under whipped state, 100 parts of starch being joined 500-600 parts, to be dissolved with mass percent concentration be in the aqueous solution of 18-25% starch granules swelling inhibitor, and temperature controls at 35-45 DEG C, do not stop to stir, obtain starch milk;
Described starch is sweet potato starch;
Described starch granules swelling inhibitor is sodium sulfate, and concentration is in aqueous 18-25%;
(2) alkalize: under whipped state, add 0.8-1.1 parts of catalyzer in starch milk, temperature controls at 35-45 DEG C, and alkalization time is 40-50min, obtains mixed solution;
Described catalyzer is sodium hydroxide;
(3) etherificate: under whipped state, keep temperature to be 35-45 DEG C, add 3.1-3.5 parts of vinyl cyanide in mixed solution, react 3.5-4h under 35-45 DEG C of conditions after, etherification reaction terminates, and obtains cyanoethyl starch mixed solution;
(4) be separated: cyanoethyl starch mixed solution is proceeded in the whizzer of band filter cloth and be separated to obtain the first cyanoethyl starch crude product;
(5) acidifying: under whipped state, the first cyanoethyl starch crude product being dissolved in 220-300 parts of mass percent concentrations is in the aqueous ethanolic solution of 81%, add 2.5-2.8 parts of Glacial acetic acid, react 45-50min under 40-45 DEG C of conditions after, acidification reaction terminates, and obtains the second cyanoethyl starch crude product after centrifugation;
(6) refining: the second cyanoethyl starch crude product to be washed, centrifugation, obtain refining cyanoethyl starch wet product;
The step of described washing, centrifugation is: with the mass percent concentration that temperature is 20-40 DEG C be 81% aqueous ethanolic solution the second cyanoethyl starch crude product is washed, washing liquid level is as the criterion with submergence cyanoethyl starch, after stirring 20min, centrifugation obtains primary purification cyanoethyl starch; Repeat above-mentioned steps 2-3 times, when filtrate pH >=5.6;
(7) dry: cyanoethyl starch wet product dry 2-3h in 80-85 DEG C of baking ovens will to be refined, obtain cyanoethyl starch.
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| CN201310173638.0A CN103214590B (en) | 2013-05-11 | 2013-05-11 | A kind of preparation method of cyanoethyl starch |
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| CN201310173638.0A CN103214590B (en) | 2013-05-11 | 2013-05-11 | A kind of preparation method of cyanoethyl starch |
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| CN105859896A (en) * | 2016-04-15 | 2016-08-17 | 蚌埠学院 | Acetyl cyanoethylated starch and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3515718A (en) * | 1967-07-13 | 1970-06-02 | Charles L Mehltretter | Hypochlorite modified cyanoethylated starch having intact granule form |
| CN102311507A (en) * | 2011-06-28 | 2012-01-11 | 郑桂富 | Preparation method of pharmaceutical adjuvant sodium carboxymethyl starch |
-
2013
- 2013-05-11 CN CN201310173638.0A patent/CN103214590B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3515718A (en) * | 1967-07-13 | 1970-06-02 | Charles L Mehltretter | Hypochlorite modified cyanoethylated starch having intact granule form |
| CN102311507A (en) * | 2011-06-28 | 2012-01-11 | 郑桂富 | Preparation method of pharmaceutical adjuvant sodium carboxymethyl starch |
Non-Patent Citations (2)
| Title |
|---|
| 氰乙基淀粉/聚乙烯醇共混膜的制备与性能研究;李楠等;《包装工程》;20080331;第29卷(第3期);第4-6页 * |
| 氰乙基淀粉制备及其纸张表面施胶性能;王卓妮等;《中国造纸》;20060430;第25卷(第4期);第9-11页 * |
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Effective date of registration: 20161026 Address after: 233030 Cao Road, Anhui, Bengbu No. 1866 Patentee after: Bengbu College Address before: 233000 Anhui city of Bengbu province Mei Lin Yuan Building 2 unit 3 No. 10 Patentee before: Zheng Guifu |
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