CN105755862A - Preparation method of carboxymethylated Semen Cassiae gum reactive dye printing paste - Google Patents
Preparation method of carboxymethylated Semen Cassiae gum reactive dye printing paste Download PDFInfo
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- CN105755862A CN105755862A CN201610249568.6A CN201610249568A CN105755862A CN 105755862 A CN105755862 A CN 105755862A CN 201610249568 A CN201610249568 A CN 201610249568A CN 105755862 A CN105755862 A CN 105755862A
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- printing paste
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- semen cassiae
- bean gum
- active dye
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
- D06P1/46—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders using compositions containing natural macromolecular substances or derivatives thereof
- D06P1/48—Derivatives of carbohydrates
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/38—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using reactive dyes
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- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Molecular Biology (AREA)
- General Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Medicinal Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention discloses a preparation method of carboxymethylated Semen Cassiae gum reactive dye printing paste.The preparation method includes adding a dissolved 45% sodium hydroxide solution into an ethanol solvent; under stirring, adding Semen Cassiae gum powder into the ethanol solvent and alkalizing for 60 minutes by controlling the temperature at about 30 DEG C; adding chloroacetic acid after alkalization is terminated, increasing the temperature to etherification temperature of 70-75 DEG C and reacting for 3.5 hours; decreasing the temperature to about 30 DEG C after reaction is terminated, and regulating a pH value to be neutral prior to washing, suction filtration, drying at 80 DEG C and grinding so as to obtain the carboxymethylated Semen Cassiae gum reactive dye printing paste.The carboxymethylated Semen Cassiae gum reactive dye printing paste with degree of substitution being 0.9-1.1 has the advantages of good net permeability, high color yield, high contour sharpness, high paste removal rate, good hand feel and excellent comprehensive printing indexes, is in line with current ecological environment-friendly development trend, and is high in industrial value since Semen Cassiae gum application is also expanded according to research results.
Description
Technical field
The present invention relates to the preparing technical field of high-substitution carboxymethyl Cassia bean gum printing paste with active dye, relate in particular to the carboxymethyl Cassia bean gum of a kind of solvent method preparation height replacement and for printing paste with active dye.
Background technology
Printing paste with active dye is all the time main based on sodium alginate thickener, along with the increase of thickener materials, sodium alginate price constantly rises, simultaneously undue exploitation Sargassum, the problem that also result in environmental protection aspect, this promotes us to develop new printing gum to replace sodium alginate.In recent years, construction features according to sodium alginate develops carboxymethyl cellulose, carboxymethyl starch, carboxymethyl guar gum, alleviate the demand pressure to sodium alginate to a certain extent, but these thickeners have applied defect mostly, carboxymethyl starch salt stability is poor, and the molecular weight of carboxymethyl cellulose and carboxymethyl guar gum is relatively big, big with cellulose affinity, the feel of PRINTED FABRIC is poor, and sodium alginate there is also the problem that tinctorial yield is not high.The thickener developing new printing quality good is necessary.
Semen Cassiae housing quality is 27%, endosperm 32%, plumule 41%, taking in the powder made by its endosperm after removing shell, main component is the mixture of polysaccharide, and relative molecular mass is about 210,000, wherein cold water solubles is 22.8%, and hot water soluble is 50.8%(80 DEG C), water-insoluble 27.93%.Cassia seeds polysaccharides have water insoluble matter content height, can not Fast-swelling and hydration, dissolution velocity slow, and viscosity is wayward, electrolyte-resistant, endurance of cutting are more weak, be easily biodegradable, be difficult to the shortcomings such as long-term preservation, aqueous solution color be deeper, limits the further application of cassia seeds polysaccharides.Therefore, cassia seeds polysaccharides is carried out chemical modification, improve its water solublity and easily biological-degradable is very important.
The research of conventional Semen Cassiae focuses primarily upon the aspects such as its composition, pharmacology, structure, extraction process and food applications, and Semen Cassiae polysaccharide chemistry study on the modification is less.At present, only having a small amount of several sections of papers and carry out the carboxymethyl-modification of cassia seeds polysaccharides using isobutanol as disperse medium, substitution value is all less, and cold water insoluble matter is more, and saturating net is poor.Research is concentrated mainly in the structure of modified technique and modified sample and the analysis of solution property, and its introducing in practical application performance is less.The present invention mainly adopts solvent method using ethanol water as disperse medium, and Cassia bean gum is carried out carboxymethyl-modification, improves its cold water soluble, saturating net and rheological property so that it is meet the requirement of printing paste with active dye.
Summary of the invention
The preparation method that it is an object of the invention to provide a kind of novel environment friendly printing paste with active dye, to alleviate the demand pressure of sodium alginate, improves the effect of printing with reactive dye product simultaneously.The saturating net of carboxymethyl Cassia bean gum of prepared high substituted degree is good, and the color strength of Printing is high, is a Green environmental protection, resourceful modification of polysaccharides thickener, it is possible to replace sodium alginate as printing paste with active dye.
A kind of preparation method of carboxymethyl Cassia bean gum printing paste with active dye, this preparation method comprises the following steps:
(1) sodium hydroxide solution that mass fraction is 45% is cooled to room temperature, join the alcoholic solution being in the ethanol of stirring to obtain sodium hydroxide, under stirring, Semen Cassiae rubber powder, quaternization 30min ~ 60min when 28 ~ 32 DEG C is added in the alcoholic solution of sodium hydroxide；
(2) quaternization adds monoxone after terminating, and is warming up to 65 DEG C ~ 75 DEG C, carries out etherification reaction 3 ~ 3.5h after stirring；
(3) after etherification reaction terminates, it is cooled to 28 ~ 32 DEG C, regulates the pH of reaction system to neutral with hydrochloric acid, after washing, sucking filtration, drying, pulverizing, obtain carboxymethyl Cassia bean gum printing paste with active dye.
With the quality of Semen Cassiae rubber powder for benchmark in described step (1), 1g Semen Cassiae rubber powder needs the volume of ethanol to be 2 ~ 2.5mL.
With the quality of Semen Cassiae rubber powder for benchmark in described step (1), 1g Semen Cassiae rubber powder needs monoxone 0.006mol ~ 0.009mol.
The ratio of described sodium hydroxide and chloroacetic amount of substance is 2 ~ 2.2:1.
In described step (1), concentration of alcohol is 95%.
The substitution value of the carboxymethyl Cassia bean gum printing paste with active dye that described step (3) obtains is 0.8 ~ 1.1.
Drying temperature in described step (3) is 80 DEG C.
Beneficial effects of the present invention: the main component of Cassia bean gum is the mixed system of polysaccharide, wherein contain more cold water insoluble matter, acid and alkali-resistance less stable, saturating net also extreme difference, do not meet the requirement of printing paste with active dye, its application performance must be improved by chemical modification.By carrying out carboxymethyl modified to Cassia bean gum, its saturating net, rheological property and solubility property have bigger improvement.Along with the increase of degree of substitution by carboxymethyl, cold water insoluble matter gradually decreases, and the saturating net performance of thickener has greatly improved, and substitution value thickener solution more than 0.9 can easily through the screen cloth of 300 orders；Along with the increase of carboxymethyl Cassia bean gum substitution value, water solublity increases, and the stamp Viscosity Index of thickener becomes big, and the change of Viscosity Index is conducive to greatly improving the speed of ROTARY SCREAM PRINTING；Due to the hydrophilic carboxymethyl functional group introduced in macromole, the crystal region of Cassia bean gum is also destroyed to a certain extent simultaneously, and enhanced dissolution rate, the uniformity of serosity is preferably；The introducing of more carboxymethyl functional group so that it is water solublity improves, and is easily washed with water removing after stamp fixation, de-paste rate is high, and the feel of fabric is better.By the printing with reactive dye Experimental comparison with sodium alginate, it has been found that the general relatively sodium alginate of the surface tinctorial yield of its stamp product is high, it is possible to substitute sodium alginate for printing trial.And Cassia bean gum abundant raw material, price are relatively cheap, can biodegradation, when environmental problem is increasingly subject to pay attention to, this invention meets the requirement of ecological, environmental protective, and this result of study has also expanded the purposes of Cassia bean gum, and industrial value is high.
Detailed description of the invention
Embodiment 1
The preparation method of the carboxymethyl Cassia bean gum printing paste with active dye of the present embodiment, comprises the following steps:
(1) by sodium hydroxide solution 53.3g(sodium hydroxide 24g that mass fraction is 45%, 0.6mol) it is cooled to room temperature, join 100mL and be in the alcoholic solution obtaining sodium hydroxide in the ethanol (95%) of stirring, under stirring, 50g Semen Cassiae rubber powder, the quaternization 60min when 28 DEG C is added in the alcoholic solution of sodium hydroxide；
(2) quaternization adds monoxone (29g, 0.3mol) after terminating, and is warming up to 65 DEG C and carries out etherification reaction 3.5h after stirring；
(3) after etherification reaction terminates, being cooled to 28 DEG C, regulate the pH of reaction system to neutral with hydrochloric acid, obtain carboxymethyl Cassia bean gum printing paste with active dye after washing, sucking filtration, 80 DEG C of drying, pulverizing, substitution value is 0.8.
Embodiment 2
The preparation method of the carboxymethyl Cassia bean gum printing paste with active dye of the present embodiment, comprises the following steps:
(1) by sodium hydroxide solution 88g(that mass fraction is 45% containing sodium hydroxide 39.6g, 0.99mol) it is cooled to room temperature, join 125mL and be in the alcoholic solution obtaining sodium hydroxide in the ethanol (95%) of stirring, under stirring, 50g Semen Cassiae rubber powder, the quaternization 30min when 32 DEG C is added in the alcoholic solution of sodium hydroxide；
(2) quaternization adds monoxone (42.5g, 0.45mol) after terminating, and is warming up to 75 DEG C, carries out etherification reaction 3h after stirring；
(3) after etherification reaction terminates, being cooled to 32 DEG C, regulate the pH of reaction system to neutral with hydrochloric acid, obtain carboxymethyl Cassia bean gum printing paste with active dye after washing, sucking filtration, 80 DEG C of drying, pulverizing, substitution value is 1.1.
Embodiment 3
The preparation method of the carboxymethyl Cassia bean gum printing paste with active dye of the present embodiment, comprises the following steps:
(1) by sodium hydroxide solution 74.7g(that mass fraction is 45% containing sodium hydroxide 33.6g, 0.84mol) it is cooled to room temperature, join 110mL and be in the alcoholic solution obtaining sodium hydroxide in the ethanol (95%) of stirring, under stirring, 50g Semen Cassiae rubber powder, the quaternization 45min when 30 DEG C is added in the alcoholic solution of sodium hydroxide；
(2) quaternization adds monoxone (37.8g, 0.4mol) after terminating, and is warming up to 70 DEG C, carries out etherification reaction 3.2h after stirring；
(3) after etherification reaction terminates, being cooled to 30 DEG C, regulate the pH of reaction system to neutral with hydrochloric acid, obtain carboxymethyl Cassia bean gum printing paste with active dye after washing, sucking filtration, 80 DEG C of drying, pulverizing, substitution value is 1.0.
Properties of sample index prepared by above-described embodiment 1 ~ 3 and for printing with reactive dye test effect in Table 1.
Properties of sample index prepared by table 1 embodiment 1 ~ 3 and for printing with reactive dye test effect
The above is only the preferred embodiments of the present invention, according to different product stamp requirements, it is possible to the carboxymethyl Cassia bean gum sample of preparation different degree of substitution, the sample printing quality of DS > 0.9 is better.
The ultimate principle of the present invention and principal character and advantages of the present invention have more than been shown and described.Skilled person will appreciate that of the industry; the present invention is not restricted to the described embodiments; described in above-described embodiment and description is that principles of the invention is described; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements both fall within the claimed scope of the invention.Claimed scope is defined by appending claims and equivalent thereof.
Claims (7)
1. the preparation method of a carboxymethyl Cassia bean gum printing paste with active dye, it is characterised in that this preparation method comprises the following steps:
(1) sodium hydroxide solution that mass fraction is 45% is cooled to room temperature, join the alcoholic solution being in the ethanol of stirring to obtain sodium hydroxide, under stirring, Semen Cassiae rubber powder, quaternization 30min ~ 60min when 28 ~ 32 DEG C is added in the alcoholic solution of sodium hydroxide；
(2) quaternization adds monoxone after terminating, and is warming up to 65 DEG C ~ 75 DEG C, carries out etherification reaction 3 ~ 3.5h after stirring；
(3) after etherification reaction terminates, it is cooled to 28 ~ 32 DEG C, regulates the pH of reaction system to neutral with hydrochloric acid, after washing, sucking filtration, drying, pulverizing, obtain carboxymethyl Cassia bean gum printing paste with active dye.
2. the preparation method of carboxymethyl Cassia bean gum printing paste with active dye according to claim 1, it is characterised in that: with the quality of Semen Cassiae rubber powder for benchmark in described step (1), 1g Semen Cassiae rubber powder needs the volume of ethanol to be 2 ~ 2.5mL.
3. the preparation method of carboxymethyl Cassia bean gum printing paste with active dye according to claim 1, it is characterised in that: with the quality of Semen Cassiae rubber powder for benchmark in described step (1), 1g Semen Cassiae rubber powder needs monoxone 0.006mol ~ 0.009mol.
4. the preparation method of carboxymethyl Cassia bean gum printing paste with active dye according to claim 1, it is characterised in that: the ratio of described sodium hydroxide and chloroacetic amount of substance is 2 ~ 2.2:1.
5. the preparation method of carboxymethyl Cassia bean gum printing paste with active dye according to claim 1, it is characterised in that: in described step (1), concentration of alcohol is 95%.
6. the preparation method of carboxymethyl Cassia bean gum printing paste with active dye according to claim 1, it is characterised in that: the substitution value of the carboxymethyl Cassia bean gum printing paste with active dye that described step (3) obtains is 0.8 ~ 1.1.
7. the preparation method of carboxymethyl Cassia bean gum printing paste with active dye according to claim 1, it is characterised in that: the drying temperature in described step (3) is 80 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610249568.6A CN105755862A (en) | 2016-04-21 | 2016-04-21 | Preparation method of carboxymethylated Semen Cassiae gum reactive dye printing paste |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610249568.6A CN105755862A (en) | 2016-04-21 | 2016-04-21 | Preparation method of carboxymethylated Semen Cassiae gum reactive dye printing paste |
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| CN105755862A true CN105755862A (en) | 2016-07-13 |
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| CN201610249568.6A Pending CN105755862A (en) | 2016-04-21 | 2016-04-21 | Preparation method of carboxymethylated Semen Cassiae gum reactive dye printing paste |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109457515A (en) * | 2018-10-26 | 2019-03-12 | 江苏华东纺织产品检测有限公司 | A kind of preparation method of velvet apple fabric digit printing thickener |
| CN110791977A (en) * | 2019-11-28 | 2020-02-14 | 四川大学 | Tara gum modified digital printing paste and preparation method thereof |
-
2016
- 2016-04-21 CN CN201610249568.6A patent/CN105755862A/en active Pending
Non-Patent Citations (3)
| Title |
|---|
| BRIJ RAJ SHARMA: "Carbamoylethylation of Cassia tora gum", 《CARBOHYDRATE POLYMERS》 * |
| 李青: "纺织品印花增稠剂研究进展", 《印染》 * |
| 柳梦思: "羧甲基决明子多糖的制备及表征", 《河北科技大学学报》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109457515A (en) * | 2018-10-26 | 2019-03-12 | 江苏华东纺织产品检测有限公司 | A kind of preparation method of velvet apple fabric digit printing thickener |
| CN110791977A (en) * | 2019-11-28 | 2020-02-14 | 四川大学 | Tara gum modified digital printing paste and preparation method thereof |
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Application publication date: 20160713 |