CN111826951A - Method for preparing modified cotton fabric with high carboxyl content by using succinic acid - Google Patents
Method for preparing modified cotton fabric with high carboxyl content by using succinic acid Download PDFInfo
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- CN111826951A CN111826951A CN201910306192.1A CN201910306192A CN111826951A CN 111826951 A CN111826951 A CN 111826951A CN 201910306192 A CN201910306192 A CN 201910306192A CN 111826951 A CN111826951 A CN 111826951A
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- succinic acid
- cotton fabric
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/184—Carboxylic acids; Anhydrides, halides or salts thereof
- D06M13/192—Polycarboxylic acids; Anhydrides, halides or salts thereof
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/68—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof
- D06M11/70—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof with oxides of phosphorus; with hypophosphorous, phosphorous or phosphoric acids or their salts
- D06M11/71—Salts of phosphoric acids
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
- D06M11/76—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon oxides or carbonates
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention relates to a method for preparing a modified cotton fabric with high carboxyl content by using succinic acid, which is characterized in that the appearance of the modified cotton fabric prepared by the method is in a shape of a brown colored fabric, wherein the carboxyl content is 0.4 millimole per gram to 1.0 millimole per gram. The succinic acid is easier to perform esterification reaction with hydroxyl in a macromolecular chain of the cotton fiber, carboxyl can be more effectively introduced into the surface of the cotton fiber, and the purpose of reducing the using amount of the carboxylic acid in the carboxylic acid modification finishing process of the cotton fiber is achieved.
Description
Technical Field
The invention relates to the technical field of chemical industry, in particular to a method for preparing a modified cotton fabric with high carboxyl content by using succinic acid.
Background
Cotton fiber is the main raw material of textile industry in China. During the production and processing of cotton textiles, a large amount of staple fibers, waste yarns, noil, and scrap material is often produced. If the waste materials are directly discarded without certain treatment, huge burden is brought to the environment, and simultaneously, a great deal of resource waste is caused. China produces and consumes a huge amount of textiles, which results in billions of tons of textile waste materials in China every year. Therefore, the waste materials are converted into usable resources as much as possible, and the waste materials are changed into valuable materials, which is a serious problem in the textile industry at present. It is worth explaining that the carboxylation modification of the waste cotton fabric is an important basic work for better utilizing the waste cotton fabric, because the carboxylation modification not only can enable the cotton fabric to have higher adsorbability to heavy metal ions and organic dyes, but also can further carry out coordination reaction with iron ions and the like to prepare the modified cotton fiber metal complex catalyst, can promote the oxidative degradation of organic pollutants in water, and has important significance for controlling the water environment pollution. In the carboxylation modification technology of cotton fabric, organic carboxylic acid such as tartaric acid and citric acid is mostly used to perform esterification treatment on the surface of the cotton fabric so as to introduce carboxyl on the surface of the cotton fabric [ see Liu G, Dong Y, Wang P, et2S2O8for dye degradation by Fe complexes fixed onpolycarboxylic acids modified waste cotton[J].Carbohydr Polym，2018：103-110.]However, the efficiency of introducing carboxyl groups on the surface of cotton fibers by tartaric acid and citric acid is not high, that is, the carboxyl group content on the surface of cotton fibers can be increased only by using high-concentration tartaric acid and citric acid, which not only causes serious waste of tartaric acid and citric acid in the reaction process, but also brings about a certain problem of environmental pollution. The invention uses succinic acid to replace tartaric acid and citric acid to carry out surface modification on the cotton fiber and introduce carboxyl, thereby not only enabling the modified cotton fiber to have higher carboxylic acid content, but also obviously reducing the dosage of organic carboxylic acid.
Disclosure of Invention
Aiming at the defects of the prior art, the technical problems to be solved by the invention are as follows: a method for preparing modified cotton fibers with high carboxyl content by using succinic acid is provided. The modified cotton fiber can improve the efficiency of introducing carboxyl on the surface of the cotton fiber, avoid the waste of organic acid in the modification process and reduce the environmental pollution. The method simplifies the carboxylic acid modification reaction process of the cotton fiber, reduces the cost, is easy to operate and is beneficial to industrial popularization.
The technical scheme for solving the problem of the modification of the cotton fiber carboxylic acid is as follows: a method for preparing modified cotton fiber with high carboxyl content by using succinic acid is characterized in that succinic acid is easier to perform esterification reaction with hydroxyl in a macromolecular chain of the cotton fiber, carboxyl is more effectively introduced on the surface of the cotton fiber than tartaric acid and citric acid, more carboxyl can be introduced on the surface of the cotton fiber by using a small amount of succinic acid, the purpose of remarkably reducing the using amount of carboxylic acid in the carboxylic acid modification reaction process of the cotton fiber is achieved, the carboxylic acid modification process of the cotton fiber is simplified, the processing cost is reduced, the environmental pollution is reduced, and the purposes of energy conservation and emission reduction are achieved. In the carboxylic acid modification reaction of the cotton fibers, when the consumption of succinic acid reaches 0.17 mol per liter, the carboxyl content of the obtained modified cotton fibers is 0.50 mmol per gram. To achieve a carboxyl content of 0.50 mmoles per gram of modified cotton fiber, more than 0.70 moles per liter of tartaric acid must be used, thus enabling a four-fifths reduction in the amount of organic carboxylic acid used.
The technical scheme for solving the technical problems of the preparation method is as follows: a method for preparing modified cotton fiber with high carboxyl content by using succinic acid is designed, and the method adopts the following process:
1. pretreatment of cotton fabric: placing the cotton fabric into an aqueous solution containing 5 grams per liter of anionic detergent and 2 grams per liter of sodium carbonate under the conditions of room temperature and stirring, treating for 30 minutes under the condition of boiling, taking out the fabric, washing for 3 times, and finally drying the fabric at 100 ℃;
2. preparing a modified solution: respectively putting succinic acid and sodium dihydrogen phosphate with specified weight into distilled water, stirring to completely dissolve, preparing an aqueous solution containing succinic acid with concentration of 20.08-80.30 g/L and sodium dihydrogen phosphate with concentration of 50 g/L, and standing the obtained mixed aqueous solution for 2-5 hours;
3. the rolling and baking treatment process comprises the following steps: modifying the pretreated cotton fabric obtained in the step 1 by using the modifying solution through a rolling and baking combined system to obtain a succinic acid modified cotton fabric;
4. and (3) post-treatment process: and (2) washing the succinic acid modified cotton fabric in the step (3) by using an anionic surfactant aqueous solution with the concentration of 2.5 grams per liter for 8 minutes at room temperature under the stirring condition, then washing the succinic acid modified cotton fabric for 3 times by using distilled water, and finally drying the succinic acid modified cotton fabric at 100 ℃ to obtain the light yellow succinic acid modified cotton fabric.
Compared with the prior art, the modified cotton fiber prepared by using succinic acid has higher carboxylic acid content. In the preparation process, the use amount of the organic carboxylic acid is greatly reduced, and the carboxyl is more effectively introduced on the surface of the cotton fiber, so that the utilization rate of the organic carboxylic acid is improved, and the content of the carboxylic acid on the surface of the modified cotton fiber is increased, so that the modification reaction process of the cotton fiber is simplified, the cost is obviously reduced, the operation is easy, and the industrial popularization is facilitated.
Drawings
FIG. 1 is the carboxyl content of the succinic acid modified cotton fabric described in examples 1-4;
FIG. 2 is a graph showing the carboxyl content of the succinic acid-modified cotton fabric described in examples 1-4 and comparative examples 1-4.
Detailed Description
The technical scheme for solving the problem of the modification of the cotton fiber carboxylic acid is as follows: a method for preparing modified cotton fiber with high carboxyl content by using succinic acid is characterized in that succinic acid is easier to perform esterification reaction with hydroxyl in a macromolecular chain of the cotton fiber, carboxyl is more effectively introduced on the surface of the cotton fiber than tartaric acid and citric acid, and more carboxyl can be introduced on the surface of the cotton fiber by using a relatively small amount of succinic acid, so that the aim of reducing the using amount of carboxylic acid in the carboxylic acid modification process of the cotton fiber is fulfilled, the carboxylic acid modification process of the cotton fiber is simplified, the processing cost is reduced, the environmental pollution is reduced, and the aims of energy conservation and emission reduction are fulfilled. In the carboxylic acid modification reaction of cotton fibers, when the consumption of succinic acid reaches 0.17 mol per liter, the carboxyl content of the obtained modified cotton fibers is 0.50 mmol per gram; to achieve a carboxyl content of 0.50 mmoles per gram of modified cotton fiber, more than 0.70 moles per liter of tartaric acid must be used, thus reducing the amount of organic carboxylic acid used by four fifths.
The method for determining the carboxyl content of the succinic acid modified cotton fiber in the embodiment of the invention comprises the following steps: firstly, 0.50 g of tartaric acid succinic acid modified cotton fiber which is cut into pieces is put into 50 ml of tartaric acid succinic acid modified cotton fiber with the concentration of 0.10In mol/l aqueous sodium hydroxide solution and allowed to react for 2 hours at room temperature under stirring and nitrogen atmosphere. Phenolphthalein indicator was then added thereto and the residual sodium hydroxide was titrated therein using a calibrated 0.10 mole per liter hydrochloric acid standard solution. The volume of the hydrochloric acid solution consumed when the red color of the aqueous solution in the system faded (titration end point) was recorded, and the surface carboxylic acid content (Q) per unit mass of the organic carboxylic acid-modified cotton fiber was calculated using the following formulaCOOHMmoles per gram):
in the formula CNaOHAnd VNaOHThe concentration (0.10 mol/l) and volume (50 ml), C, of the aqueous sodium hydroxide solution, respectivelyHClConcentration of hydrochloric acid standard solution (0.10 mol/l), VHClIs the volume (ml) of hydrochloric acid standard solution consumed by titration, and m is the mass (0.50 g) of the organic carboxylic acid modified cotton fiber.
Specific embodiments of the invention are described below, but the claims of the invention are not limited to these specific embodiments:
example 1
1. Pretreatment of cotton fabric: placing the cotton fabric into an aqueous solution containing 5 grams per liter of anionic detergent and 2 grams per liter of sodium carbonate at room temperature under stirring, treating for 30 minutes under the condition of boiling, taking out and rinsing the fabric for 3 times, and finally drying the fabric at 100 ℃;
2. preparing a modified solution: respectively putting succinic acid and sodium dihydrogen phosphate with specified weight into distilled water, stirring to completely dissolve, preparing an aqueous solution containing 20.08 grams of succinic acid per liter and 50 grams of sodium dihydrogen phosphate per liter, and finally standing the obtained mixed aqueous solution for 2 to 5 hours;
3. the rolling and baking treatment process comprises the following steps: modifying the pretreated cotton fabric obtained in the step 1 of the rolling and baking combined system by using the modifying solution to obtain a succinic acid modified cotton fabric;
4. and (3) post-treatment process: under the conditions of room temperature and stirring, firstly, washing the modified cotton fabric by using an anionic surfactant aqueous solution with the concentration of 2.5 grams per liter for 8 minutes, then taking out the cotton fabric, then washing the cotton fabric by using distilled water for 3 times, and finally drying the cotton fabric at 100 ℃ to obtain light yellow succinic acid modified cotton fabric, wherein the carboxylic acid content of the light yellow succinic acid modified cotton fabric is 0.50 millimole per gram.
Example 2
1. The process is the same as step 1 in example 1;
2. setting the concentration of succinic acid to be 40.15 g/L, and the other processes are the same as the step 2 in the embodiment 1;
3. the process is the same as step 3 in example 1;
4. the process was the same as in step 4 of example 1 to give succinic acid modified cotton fabric with a carboxylic acid content of 0.64 mmole per gram.
Example 3
1. The process is the same as step 1 in example 1;
2. setting the concentration of succinic acid to 60.23 g/L, and the other processes are the same as the step 2 in the example 1;
3. the process is the same as step 3 in example 1;
4. the process was the same as in step 4 of example 1 to give succinic acid modified cotton fabric with a carboxylic acid content of 0.70 mmole per gram.
Example 4
1. The process is the same as step 1 in example 1;
2. setting the concentration of succinic acid to be 80.30 grams per liter, and the other processes are the same as the step 2 in the embodiment 1;
3. the process is the same as step 3 in example 1;
4. the process was the same as in step 4 of example 1 to give succinic acid modified cotton fabric with a carboxylic acid content of 0.78 mmole per gram.
Comparative example
This example is a comparative example of effect. The preparation method of the carboxylic acid modified cotton fabric by using tartaric acid instead of succinic acid comprises the following steps:
comparative example 1
1. The process is the same as step 1 in example 1;
2. preparing a modified solution: respectively putting tartaric acid and sodium dihydrogen phosphate with specified weight into distilled water, stirring to completely dissolve, preparing aqueous solution containing tartaric acid with concentration of 11.8 g per liter and sodium dihydrogen phosphate with concentration of 50 g per liter, and standing the obtained mixed aqueous solution for 2-5 hours;
3. the process is the same as step 3 in example 1;
4. the procedure was the same as in step 4 of example 1, giving a carboxylic acid content of 0.11 mmole per gram of tartaric acid-modified cotton fabric.
Example 2
1. The process is the same as step 1 in example 1;
2. the tartaric acid concentration is set to be 51.03 grams per liter, and other processes are the same as the step 2 in the example 1;
3. the process is the same as step 3 in example 1;
4. the procedure was the same as in step 4 of example 1, giving a carboxylic acid content of 0.24 mmole per gram of tartaric acid-modified cotton fabric.
Example 3
1. The process is the same as step 1 in example 1;
2. the tartaric acid concentration was set at 76.55 g/l, and the other processes were the same as in step 2 of example 1;
3. the process is the same as step 3 in example 1;
4. the procedure was identical to step 4 of example 1, giving a carboxylic acid content of 0.34 mmole per gram of tartaric acid-modified cotton fabric.
Example 4
1. The process is the same as step 1 in example 1;
2. the tartaric acid concentration was set at 102.07 g/l, and the other processes were the same as in step 2 of example 1;
3. the process is the same as step 3 in example 1;
4. the procedure was the same as in step 4 of example 1, giving a carboxylic acid content of 0.45 mmole per gram of tartaric acid-modified cotton fabric.
FIG. 1 shows that the carboxyl content of the resulting modified cotton fiber was 0.50 mmole per gram when succinic acid was used in an amount of 0.17 moles per liter; the carboxyl content of the modified cotton fiber is almost linearly increased along with the increase of the consumption of the succinic acid. When the amount of succinic acid used reaches 0.68 mol per liter, the carboxyl content of the obtained modified cotton fiber is 0.78 mmol per gram.
Figure 2 shows that the carboxylic acid content of succinic acid modified cotton fabric with the same molar concentration is significantly higher than that of tartaric acid modified cotton fabric, especially at low concentrations this trend is more pronounced. The results show that when succinic acid is used for replacing tartaric acid to carry out modification treatment on cotton fabrics, the use amount of organic carboxylic acid is remarkably reduced, carboxyl is more effectively introduced to the surfaces of cotton fibers, the utilization rate of the organic carboxylic acid is improved, and the content of the carboxylic acid on the surfaces of the modified cotton fibers is increased.
As can be seen from a comparison of fig. 1 and 2, the amount of organic carboxylic acid can be significantly saved when succinic acid is used instead of tartaric acid for the modification of cotton fiber, and particularly, the amount of organic carboxylic acid can be reduced by at least four fifths when the modification is performed using low concentration of organic carboxylic acid.
The above-mentioned embodiments only express the embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several modifications can be made without departing from the inventive concept, and these modifications belong to the protective scope of the invention.
Claims (1)
1. A method for preparing modified cotton fabric with high carboxyl content by using succinic acid adopts the following process:
step 1: pretreatment of cotton fabric: placing the cotton fabric in an aqueous solution containing 5.0 g per liter of anionic detergent and 2.0 g per liter of sodium carbonate at room temperature under stirring, treating for 30 minutes under boiling, taking out the fabric, washing for 3 times, and drying at 100 ℃;
step 2: preparing a modified solution: respectively putting succinic acid and sodium dihydrogen phosphate with specified weight into distilled water, stirring to completely dissolve, preparing aqueous solution containing succinic acid with concentration of 11.8-82.6 g/L and sodium dihydrogen phosphate with concentration of 50 g/L, and standing the obtained mixed aqueous solution for 2-5 hours;
and step 3: the rolling and baking treatment process comprises the following steps: modifying the pretreated cotton fabric obtained in the step 1 by using the modifying solution through a rolling and baking combined system to obtain a succinic acid modified cotton fabric;
and 4, step 4: and (3) post-treatment process: and (2) washing the succinic acid modified cotton fabric obtained in the step (3) for 8 minutes by using an anionic surfactant aqueous solution with the concentration of 2.5 grams per liter at room temperature under the stirring condition, then washing the succinic acid modified cotton fabric for 3 times by using distilled water, and finally drying the succinic acid modified cotton fabric at 100 ℃ to obtain the light yellow succinic acid modified cotton fabric.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1039456A (en) * | 1988-06-16 | 1990-02-07 | 美国政府(美国商务部代表) | With polybasic carboxylic acid COTTON FABRIC is carried out formaldehyde-free durable and press technology and the employed catalyst that scalds arrangement |
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| CN105921174A (en) * | 2016-05-20 | 2016-09-07 | 天津工业大学 | Recycling method of waste cellulose fabric |
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2019
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Patent Citations (6)
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|---|---|---|---|---|
| CN1039456A (en) * | 1988-06-16 | 1990-02-07 | 美国政府(美国商务部代表) | With polybasic carboxylic acid COTTON FABRIC is carried out formaldehyde-free durable and press technology and the employed catalyst that scalds arrangement |
| US6471824B1 (en) * | 1998-12-29 | 2002-10-29 | Weyerhaeuser Company | Carboxylated cellulosic fibers |
| CN101591854A (en) * | 2009-06-23 | 2009-12-02 | 东华大学 | A kind of method for sorting of cellulosic fabric nano durable super hydrophobicity |
| CN104174441A (en) * | 2014-09-09 | 2014-12-03 | 天津工业大学 | Low-cost and environment-friendly type modified cotton fiber iron complex catalyst and preparation method of catalyst |
| CN104358116A (en) * | 2014-10-14 | 2015-02-18 | 东华大学 | Polybasic carboxylic acid non-ironing process washing-free method adopting urea as additive |
| CN105921174A (en) * | 2016-05-20 | 2016-09-07 | 天津工业大学 | Recycling method of waste cellulose fabric |
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