Method for preparing fancy cashmere yarn by using colored spun fibers

文档序号:1932245 发布日期:2021-12-07 浏览:27次 中文

阅读说明:本技术 一种利用色纺纤维制备花式羊绒纱的方法 (Method for preparing fancy cashmere yarn by using colored spun fibers ) 是由 陈刚 薛惊理 秦保新 徐媛媛 候会 于 2021-09-14 设计创作,主要内容包括:本发明公开了一种利用色纺纤维制备花式羊绒纱的方法,涉及纺纱技术领域,具体包括:S1:先对羊绒毛进行染色,制成均匀的毛条,投入生产,通过精纺或半精纺做成粗纱;S2:花捻PAFA生产,采用花捻机对羊绒粗纱进行花式纱生产得到花式羊绒纱线;S3:拉毛,对做好的花式羊绒纱线进行拉毛;S4:蒸纱,对拉毛后的纱线进行蒸纱;S5:倒筒,蒸完的纱线通过倒成筒纱即得产品。本发明提供的方法大大缩短了工艺流程,降低了成本,提高了纱线出货的效率,避免了色差问题,具有节能减排的优势;且制得的花式羊绒纱力学性能优异,柔软度良好,颜料在织物上的色牢度高,上染率更佳。(The invention discloses a method for preparing fancy cashmere yarns by utilizing colored spun fibers, which relates to the technical field of spinning and specifically comprises the following steps: s1: dyeing cashmere wool to prepare uniform wool tops, putting the wool tops into production, and preparing the wool tops into rough yarns through spinning or semi-spinning; s2: producing the fancy yarn PAFA, namely producing fancy yarn on the cashmere roving by adopting a fancy twisting machine to obtain fancy cashmere yarn; s3: napping, namely napping the finished fancy cashmere yarn; s4: steaming yarn, namely steaming the napped yarn; s5: and (5) rewinding, and rewinding the steamed yarns into cone yarns to obtain the finished product. The method provided by the invention greatly shortens the process flow, reduces the cost, improves the yarn delivery efficiency, avoids the problem of chromatic aberration, and has the advantages of energy conservation and emission reduction; the prepared fancy cashmere yarn has excellent mechanical property, good softness, high color fastness of the pigment on the fabric and better dye uptake.)

1. A polymeric hybrid pigment comprising:

a pigment/polymer composite material, wherein the polymer is coated on the surface of the pigment;

the polymer is styrene-acrylic resin, and the crosslinking monomer of the polymer comprises 4- [ (2R) -3, 4-dihydro-7-hydroxy-2H-1-benzopyran-2-yl ] -3- (3-methyl-2-butylene-1-yl) -1, 2-benzenediol.

2. A method of preparing the polymeric hybrid pigment of claim 1, comprising preparing the pigment/polymer composite by an emulsion miniemulsion process.

3. A method for preparing fancy cashmere yarns by utilizing colored spun fibers comprises the following specific processes: dyeing cashmere wool, twisting, napping, steaming yarn and rewinding.

4. A method for making fancy cashmere yarns using dyed fibers according to claim 3, characterized in that: the pigment used in the dyeing process comprises the polymeric hybrid pigment of claim 1.

5. A method for making fancy cashmere yarns using dyed fibers according to claim 3, characterized in that: after dyeing, soft finishing is carried out; and (4) adopting a softening agent for dipping treatment.

6. A method for making fancy cashmere yarns using dyed fibers according to claim 5, wherein: the softening agent is organic silicone oil; the raw materials of the organic silicone oil comprise PMHS and N- (methoxymethyl) methacrylamide.

7. A method for making fancy cashmere yarns using dyed fibers according to claim 6, wherein: the organic silicone oil raw material also comprises apigenin.

8. Use of the polymeric hybrid pigment of claim 1 in textile coloration, ink printing and rubber plastic preparation.

9. Use according to claim 8, characterized in that: the use of the 4- [ (2R) -3, 4-dihydro-7-hydroxy-2H-1-benzopyran-2-yl ] -3- (3-methyl-2-butene-1-yl) -1, 2-benzenediol to enhance the light, friction and wash fastness of pigments on fabrics.

10. Use of the silicone oil of claim 7 for enhancing the mechanical properties and smoothness of cashmere yarns.

Technical Field

The invention belongs to the technical field of spinning, and particularly relates to a method for preparing fancy cashmere yarns by utilizing colored spun fibers.

Background

The colored spun yarn is used for dyeing fibers into colored fibers, and hazy three-dimensional effect and texture which cannot be achieved by white blank dyeing can be achieved. The colored spun yarn has no pollution in use, and can control color difference to the maximum extent. Therefore, the color is soft and fashionable, the color spinning yarn can be used for small-batch multi-variety flexible production, and is increasingly applied to middle-high-grade clothing products. Compared with the traditional process of adopting the dyeing after spinning, the performance of the colored spun yarn is superior to that of other textile products, and the colored spun yarn has stronger market competitiveness and better market prospect.

Although the production capacity of the Chinese textile industry occupies the first position of the world for many years, the Chinese textile fiber has limited resources and has heavy tasks of saving energy, reducing emission, reducing consumption and reducing environmental pollution. Meanwhile, international clothing and home textile products have entered a new era of ecology, safety and health care, all of which put forward higher requirements on the traditional textile industry of China, and the whole industry needs to be cut in by scientific and technological innovation to research and implement the series of problems. At present, along with the wide application of information technology, the level of textile machinery and mechanical and electrical integration is continuously improved, the introduction and learning of foreign advanced equipment, and the overall technical level of the textile industry is continuously improved.

Compared with the traditional process of 'spinning before and then dyeing', the colored spun yarn serving as a subdivision sub-industry of the textile industry shortens the production flow of subsequent processing enterprises, reduces the production cost, has higher added value, especially solves the problem of great pollution of the traditional dyeing and finishing industry in a breakthrough manner, and greatly reduces the energy consumption and the environmental damage because of the new technical means of 'spinning before and after' dyeing. The spun-dyed yarn is generally spun by mixing two or more kinds of fibers with different colors or different properties, and the process is mainly a physical mixing process. The colored spun yarn has rich colors, clear layers, strong three-dimensional sense of colors and good color light consistency, and the cloth cover presents the characteristics of multiple colors, soft hand feeling and plump surface feeling after being woven into cloth.

The core technology in the field of color spinning industry is mainly embodied in the aspects of sewage treatment, energy conservation and emission reduction, cotton fiber dyeing, new variety development and the like. If the fabric occupies a place in the color spinning industry, the third problem is a difficult problem to solve in the technical aspect.

Disclosure of Invention

The invention aims to provide a method for preparing fancy cashmere yarns by utilizing colored spun fibers, which greatly shortens the process flow, reduces the cost, improves the delivery efficiency of the yarns, avoids the problem of chromatic aberration, and has the advantages of energy conservation and emission reduction; the prepared fancy cashmere yarn has excellent mechanical property, good softness, high color fastness of the pigment on the fabric and better dye uptake.

The technical scheme adopted by the invention for realizing the purpose is as follows:

a polymeric hybrid pigment comprising: a pigment/polymer composite; the polymer is coated on the surface of the pigment;

the polymer is styrene-acrylic resin, and the crosslinking monomer of the polymer comprises 4- [ (2R) -3, 4-dihydro-7-hydroxy-2H-1-benzopyran-2-yl ] -3- (3-methyl-2-butylene-1-yl) -1, 2-benzenediol. According to the invention, 4- [ (2R) -3, 4-dihydro-7-hydroxy-2H-1-benzopyran-2-yl ] -3- (3-methyl-2-butylene-1-yl) -1, 2-benzenediol modified styrene-acrylic resin is used as a polymer to wrap the pigment, so that the large-scale aggregation phenomenon among pigment particles can be effectively avoided; the existence of 4- [ (2R) -3, 4-dihydro-7-hydroxy-2H-1-benzopyran-2-yl ] -3- (3-methyl-2-butylene-1-yl) -1, 2-benzenediol can effectively improve the coating rate of the polymer to pigment particles, further improve the dispersion stability of the hybrid pigment in a water phase, obviously enhance the ultrasonic dispersion stability and the storage stability of the hybrid pigment, and enable the pigment to fully exert the coloring potential; when the dye is applied to a textile dyeing process, the coloring strength and the covering power of the pigment on the textile are greatly enhanced, the grades of the light fastness, the rubbing fastness and the washing fastness are obviously improved, and the color fastness of the dyed textile is effectively improved; and can further improve the dye uptake of the pigment. In addition, the mechanical property of the fabric can be improved to a certain extent, and the breaking strength of the fabric can be enhanced.

The preparation method of the polymer hybrid pigment comprises the step of preparing the pigment/polymer composite material by a miniemulsion method.

Further, the preparation method of the polymer hybrid pigment specifically comprises the following steps:

1) removing substances such as salt and the like of industrial grade pigment crystals by adopting a washing method;

2) mixing and stirring the cleaned pigment crystal dispersion liquid, an emulsifier OP-10 and water for 20-40 min, adding St, BA and 4- [ (2R) -3, 4-dihydro-7-hydroxy-2H-1-benzopyran-2-yl ] -3- (3-methyl-2-butylene-1-yl) -1, 2-benzenediol, adding HD and SDS, mixing and stirring for pre-emulsification for 0.5-1H, and then carrying out ultrasonic treatment for 10-20 min under the power of 130-150W; and adding an initiator KPS, keeping the temperature of the water bath at 75-80 ℃, stirring and reacting for 8-12 h, centrifuging, washing and drying to obtain the polymer hybrid pigment.

According to the invention, the mass ratio of the pigment crystal dispersion liquid, OP-10 and water is 1: 0.2-0.35: 60-70 parts of; st, BA and 4- [ (2R) -3, 4-dihydro-7-hydroxy-2H-1-benzopyran-2-yl ] -3- (3-methyl-2-buten-1-yl) -1, 2-benzenediol in a mass ratio of 1: 0.9-1.4: 0.8 to 1.2; the mass ratio of St, HD and SDS is 1: 0.05-0.15: 0.03 to 0.08; the ratio of the pigment crystal dispersion liquid to the total mass of the monomers is 1: 1.5 to 4.

A method for preparing fancy cashmere yarns by utilizing colored spun fibers comprises the following specific processes: dyeing cashmere wool, twisting, napping, steaming yarn and rewinding.

Furthermore, the method for preparing the fancy cashmere yarn by using the colored spinning fiber specifically comprises the following steps:

s1: dyeing 1/3 cashmere wool, mixing with the rest 2/3 cashmere wool to prepare uniform wool tops, putting the wool tops into production, and preparing roving through spinning or semi-spinning;

s2: producing the fancy yarn PAFA, namely producing fancy yarn on the cashmere roving by adopting a fancy twisting machine to obtain fancy cashmere yarn;

s3: napping, namely napping the finished fancy cashmere yarn;

s4: steaming yarn, namely steaming the napped yarn;

s5: and (5) rewinding, and rewinding the steamed yarns into cone yarns to obtain the finished product.

In the preparation method of the fancy cashmere yarn, the yarn count can be controlled from the source in the fancy twisting production; the napping operation makes the yarn soft and warm; and then steaming the napped yarn, so that the internal stress of the yarn can be effectively eliminated, the twist is balanced, the strength of the yarn is improved, the quality of the yarn is improved, and the productivity is increased. The whole preparation process shortens the process flow: the colored spun fibers are used for producing the fancy cashmere yarns, so that the process of producing, dyeing and reproducing the yarns is omitted, manpower and material resources are greatly saved, and the efficiency of delivering the yarns is improved; the yarn count deviation and the color difference are reduced, and the problem of the color difference caused by the yarn count deviation and uneven dyeing caused by dyeing is solved; the spinning technology has the obvious advantages of energy conservation, emission reduction and environmental protection, the colored yarns only dye 1/3 fibers, 100% of colored yarns can be obtained through blending, compared with other industries, the spinning technology to weaving the fabric can reduce wastewater discharge by nearly 1/3, and the spinning technology by using the dope dyed fibers completely realizes zero wastewater pollution discharge and responds to carbon neutralization calls advocated by the nation.

According to the present invention, the pigment used in the dyeing process includes the above-mentioned polymeric hybrid pigment.

Further, the dyeing process comprises:

(1) soaking the cashmere wool in water for 3-6 min, taking out and wringing for later use;

(2) the pigment concentration owf (mass ratio of the pigment to the sheep wool) is 4.8-9.6%, the dyeing temperature is 70-90 ℃, the pH value is 4-6, and the bath ratio is 1: 15-30, dyeing for 40-60 min, taking out the dyed sheep villi, washing with acid soap, washing with water, and drying.

According to the invention, after dyeing, a softening finish, i.e. a treatment of impregnation with a softening agent, is also carried out.

Further, the softening agent impregnation treatment specifically comprises the following steps:

taking organic silicone oil, and mixing the organic silicone oil and the organic silicone oil according to a volume ratio of 1: 1-1.5, stirring for 15-20 min to obtain uniform emulsion, filtering, and performing soft finishing on dyed sheep down through a dipping process, wherein the using amount of the emulsion is 1.0-3 wt% (on the weight of the fabric), and the bath ratio is 1: 4-7, finishing for 10-20 min at 30-35 ℃; and finally, dehydrating, drying at 100-120 ℃ and shaping.

According to the invention, the softening agent is organic silicone oil; the raw materials of the organic silicone oil comprise PMHS and N- (methoxymethyl) methacrylamide.

According to the invention, the silicone oil raw material also comprises apigenin. According to the invention, the parsley brain is used as a cross-linking agent and is subjected to composite cross-linking with PMHS and N- (methoxymethyl) methacrylamide to prepare the organic silicone oil, and the organic silicone oil is used as a softening agent applied to a fabric softening finishing process, so that the surface performance of fibers can be effectively improved, and the flexibility and smoothness of cashmere fibers are enhanced, so that the fibers are easier to be carded and drafted in the spinning process; the color fastness of the dyed fabric can be further improved to a certain extent, and the grades of the light fastness and the fastness to washing and fading are enhanced; the mechanical property of the fabric can be effectively enhanced, and the breaking strength and the breaking elongation are obviously improved.

Further, a preparation method of the organic silicone oil comprises the following steps:

adding an isopropanol solution of PMHS and 0.5% chloroplatinic acid into a four-neck flask, connecting a condenser pipe, introducing nitrogen for 5-8 min, slowly heating, stirring and heating to 80-85 ℃, slowly adding a toluene solution dissolved with N- (methoxymethyl) methacrylamide, after dropwise addition is completed within 1-2 h, heating the system to 100-110 ℃, and reacting for 10-12 h; and finally, slowly reducing the temperature to room temperature, carrying out reduced pressure distillation, sequentially dissolving and precipitating trichloromethane and absolute ethyl alcohol, dissolving the precipitate in n-hexane, centrifuging, carrying out reduced pressure distillation, and repeatedly operating for 3-5 times to obtain the organic silicon oil.

Or the like, or, alternatively,

adding an isopropanol solution of PMHS and 0.5% chloroplatinic acid into a four-neck flask, connecting a condenser pipe, introducing nitrogen for 5-8 min, slowly heating, stirring and heating to 80-85 ℃, slowly adding a toluene solution in which apigenin is dissolved, dropwise adding within 1-2 h, heating the system to 100-110 ℃, and reacting for 4-5 h; slowly adding a toluene solution dissolved with N- (methoxymethyl) methacrylamide, after dropwise adding within 1-2 h, heating the system to 100-110 ℃, and reacting for 10-12 h; and finally, slowly reducing the temperature to room temperature, carrying out reduced pressure distillation, sequentially dissolving and precipitating trichloromethane and absolute ethyl alcohol, dissolving the precipitate in n-hexane, centrifuging, carrying out reduced pressure distillation, and repeatedly operating for 3-5 times to obtain the organic silicon oil.

According to the invention, the molar ratio of PMHS, carveol and N- (methoxymethyl) methacrylamide was 1: 0.75-0.9: 0.6 to 0.8; the dosage of the chloroplatinic acid catalyst is 55-60 mu g/g (relative to the total amount of the reaction monomers).

According to the invention, the organic silicone oil is used for enhancing the mechanical property and the smoothness of the cashmere yarn.

The invention also discloses application of the polymer hybrid pigment in textile coloring, ink printing and rubber plastic preparation.

The invention also discloses the application of the 4- [ (2R) -3, 4-dihydro-7-hydroxy-2H-1-benzopyran-2-yl ] -3- (3-methyl-2-butylene-1-yl) -1, 2-benzenediol in enhancing the light fastness, the rubbing fastness and the color fastness to washing and fading of the pigment on the fabric.

Compared with the prior art, the invention has the following beneficial effects:

the method for preparing the fancy cashmere yarn by using the colored spun fibers shortens the process flow, greatly saves manpower and material resources and improves the efficiency of yarn delivery; the problems of yarn count deviation caused by dyeing and color difference caused by uneven dyeing are avoided; has obvious advantages in energy conservation, emission reduction and environmental protection, and responds to the call of carbon neutralization advocated by the nation. The dyeing process adopts 4- [ (2R) -3, 4-dihydro-7-hydroxy-2H-1-benzopyran-2-yl ] -3- (3-methyl-2-butylene-1-yl) -1, 2-benzenediol modified styrene-acrylic resin as a polymer to wrap the pigment, so that the coating rate of the polymer on pigment particles can be effectively improved, the dispersion stability of the hybrid pigment in a water phase is further improved, and the ultrasonic dispersion stability and the storage stability of the hybrid pigment are remarkably enhanced; the color fastness of the pigment on the fabric is greatly enhanced, and the grades of the light fastness, the rubbing fastness and the washing fastness are obviously improved; the dye uptake of the pigment is obviously improved; and also improves the mechanical properties of the fabric. In addition, the soft finishing agent organic silicone oil is added to the carvone, so that after the dyed fibers are finished, the smoothness of the cashmere fibers is effectively enhanced, the color fastness of the dyed fabrics is further improved, and the grades of the light fastness and the fastness to washing and fading are enhanced; and the mechanical property of the fabric can be effectively enhanced, and the breaking strength and the breaking elongation are obviously improved.

Therefore, the invention provides a method for preparing fancy cashmere yarns by utilizing colored spun fibers, which greatly shortens the process flow, reduces the cost, improves the delivery efficiency of the yarns, avoids the problem of chromatic aberration, and has the advantages of energy conservation and emission reduction; the prepared fancy cashmere yarn has excellent mechanical property, good softness, high color fastness of the pigment on the fabric and better dye uptake.

Drawings

FIG. 1 is a TEM test of pigment Red 170 of the present invention;

FIG. 2 is the TEM test results of the polymer hybrid pigment of example 1 of the present invention;

FIG. 3 shows the results of mid-IR spectroscopy in test example 1 of the present invention;

FIG. 4 shows the results of the ultrasonic dispersion stability test of the polymer hybrid pigment prepared in comparative example 1 according to the present invention;

FIG. 5 shows the results of the ultrasonic dispersion stability test of the polymer hybrid pigment prepared in example 1 of the present invention;

FIG. 6 shows the results of the storage stability spectrum test of the polymer hybrid pigment of test example 1 of the present invention.

Detailed Description

The technical solution of the present invention is further described in detail below with reference to the following detailed description and the accompanying drawings:

the industrial pigment crystal used in the examples of the present invention was a pigment red 170 crystal dispersion, which was obtained from Liliaceae ryan pigment, Inc. in Hangzhou.

Example 1:

preparation of polymeric hybrid pigment:

1) the method for removing substances such as salt and the like of industrial grade pigment crystals by adopting a washing method comprises the following steps: carrying out centrifugal washing on the pigment crystal dispersion liquid sequentially at 10000r/min, 8000r/min and 5000r/min, and centrifuging for 8min each time;

2) taking the cleaned pigment crystal dispersion liquid, an emulsifier OP-10 and water (the mass ratio of the three is 1: 0.28: 64) mixing and stirring for 30min, adding St, BA and 4- [ (2R) -3, 4-dihydro-7-hydroxy-2H-1-benzopyran-2-yl ] -3- (3-methyl-2-butylene-1-yl) -1, 2-benzenediol (the mass ratio of the three is 1: 1.2: 1) wherein the ratio of the total mass of the pigment crystal dispersion liquid to the total mass of the monomers is 1: 3.1, adding HD and SDS (the mass ratio of St to HD to SDS is 1: 0.11: 0.06), mixing, stirring and pre-emulsifying for 1h, and then carrying out ultrasonic treatment for 20min under the power of 150W; and adding an initiator KPS, keeping the temperature of a water bath at 78 ℃, stirring and reacting for 10 hours, centrifuging, washing and drying to obtain the polymer hybrid pigment.

Preparation of the organic silicone oil:

adding PMHS and an isopropanol solution of 0.5% chloroplatinic acid (the dosage of the chloroplatinic acid is 58 mu g/g) into a four-neck flask, connecting a condensation pipe, introducing nitrogen for 6min, slowly heating and stirring to raise the temperature to 80 ℃, and slowly adding a toluene solution dissolved with N- (methoxymethyl) methacrylamide, wherein the molar ratio of the PMHS to the N- (methoxymethyl) methacrylamide is 1: 0.7, after the dropwise addition is finished within 2 hours, raising the temperature of the system to 105 ℃, and reacting for 11 hours; and finally, slowly reducing the temperature to room temperature, carrying out reduced pressure distillation, sequentially dissolving and precipitating the chloroform and the absolute ethyl alcohol, dissolving the precipitate in n-hexane, centrifuging, carrying out reduced pressure distillation, and repeatedly operating for 5 times to obtain the modified silicone oil.

A method for preparing fancy cashmere yarns by utilizing colored spun fibers comprises the following specific steps:

s1: dyeing 1/3 cashmere wool, mixing with the rest 2/3 cashmere wool to prepare uniform wool tops, putting the wool tops into production, and preparing roving through semi-worsted spinning;

s2: producing the fancy yarn PAFA, namely producing fancy yarn on the cashmere roving by adopting a fancy twisting machine to obtain fancy cashmere yarn;

s3: napping, namely napping the finished fancy cashmere yarn;

s4: steaming yarn, namely steaming the napped yarn;

s5: and (5) rewinding, and rewinding the steamed yarns into cone yarns to obtain the finished product.

Wherein the content of the first and second substances,

the dyeing process specifically comprises the following steps:

(1) soaking cashmere wool in water for 5min, taking out and wringing for later use;

(2) the pigment concentration owf (mass ratio of pigment to sheep wool) was 6.5%, the dyeing temperature was 75 ℃, the pH was 5.5, the bath ratio was 1: 20.5, dyeing for 50min, taking out the dyed sheep villi, washing with acid soap, washing with water, and drying.

According to the invention, after dyeing, a softening finish, i.e. a treatment of impregnation with a softening agent, is also carried out.

Further, the softening agent impregnation treatment specifically comprises the following steps:

taking organic silicone oil, and mixing the organic silicone oil and the organic silicone oil according to a volume ratio of 1: 1.5, stirring for 20min to obtain uniform emulsion, filtering, and performing soft finishing on dyed sheep hair by using a dipping process, wherein the using amount of the emulsion is 2.4 wt% (based on the weight of the fabric), and the bath ratio is 1: finishing at 6, 32 ℃ for 20 min; and finally, dehydrating, drying at 100 ℃ and shaping.

Example 2:

the preparation of the polymeric hybrid pigment differed from example 1 in that: the mass ratio of the pigment crystal dispersion liquid to the OP-10 to the water is 1: 0.22: 62.5; st, BA and 4- [ (2R) -3, 4-dihydro-7-hydroxy-2H-1-benzopyran-2-yl ] -3- (3-methyl-2-buten-1-yl) -1, 2-benzenediol in a mass ratio of 1: 1.3: 0.84; the mass ratio of St, HD and SDS is 1: 0.06: 0.07; the ratio of the pigment crystal dispersion liquid to the total mass of the monomers is 1: 2.4.

the silicone oil was prepared as in example 1.

A method for preparing fancy cashmere yarn using colored spun fiber was the same as in example 1.

Example 3:

the preparation of the polymeric hybrid pigment differed from example 1 in that: the mass ratio of the pigment crystal dispersion liquid to the OP-10 to the water is 1: 0.32: 61.5; st, BA and 4- [ (2R) -3, 4-dihydro-7-hydroxy-2H-1-benzopyran-2-yl ] -3- (3-methyl-2-buten-1-yl) -1, 2-benzenediol in a mass ratio of 1: 0.95: 1.1; the mass ratio of St, HD and SDS is 1: 0.14: 0.05; the ratio of the pigment crystal dispersion liquid to the total mass of the monomers is 1: 1.6.

the silicone oil was prepared as in example 1.

A method for preparing fancy cashmere yarn using colored spun fiber was the same as in example 1.

Example 4:

the preparation of the polymeric hybrid pigment differed from example 1 in that: the mass ratio of the pigment crystal dispersion liquid to the OP-10 to the water is 1: 0.3: 69.5; st, BA and 4- [ (2R) -3, 4-dihydro-7-hydroxy-2H-1-benzopyran-2-yl ] -3- (3-methyl-2-buten-1-yl) -1, 2-benzenediol in a mass ratio of 1: 1: 1.2; the mass ratio of St, HD and SDS is 1: 0.15: 0.07; the ratio of the pigment crystal dispersion liquid to the total mass of the monomers is 1: 3.9.

the silicone oil was prepared as in example 1.

A method for preparing fancy cashmere yarn using colored spun fiber was the same as in example 1.

Example 5:

the preparation of the polymeric hybrid pigment was the same as in example 1.

Preparation of the organic silicone oil:

adding PMHS and an isopropanol solution of 0.5% chloroplatinic acid (the dosage of the chloroplatinic acid is 58 mug/g) into a four-neck flask, connecting a condensation pipe, introducing nitrogen for 6min, slowly heating, stirring, heating to 80 ℃, slowly adding a toluene solution dissolved with apigenin, after dropwise addition is completed within 2h, heating the system to 105 ℃, and reacting for 5 h; slowly adding a toluene solution dissolved with N- (methoxymethyl) methacrylamide, finishing dropwise adding within 2h, raising the system temperature to 105 ℃, and reacting for 11 h; and finally, slowly reducing the temperature to room temperature, carrying out reduced pressure distillation, sequentially dissolving and precipitating the chloroform and the absolute ethyl alcohol, dissolving the precipitate in n-hexane, centrifuging, carrying out reduced pressure distillation, and repeatedly operating for 5 times to obtain the modified silicone oil. The reaction process finds that the molar ratio of PMHS, carveol and N- (methoxymethyl) methacrylamide was 1: 0.82: 0.7.

a method for preparing fancy cashmere yarn using colored spun fiber was the same as in example 1.

Example 6:

the preparation of the polymeric hybrid pigment differed from example 1 in that: the preparation process does not add 4- [ (2R) -3, 4-dihydro-7-hydroxy-2H-1-benzopyran-2-yl ] -3- (3-methyl-2-butylene-1-yl) -1, 2-benzenediol.

The silicone oil was prepared as in example 5.

A method for preparing fancy cashmere yarn using colored spun fibers is different from example 1 in that: the pigment used in the dyeing process of step S1 was obtained in this example.

Example 7:

a method for preparing fancy cashmere yarns by utilizing colored spun fibers comprises the following specific steps:

s1: dyeing 1/3 cashmere wool (conventional dyeing process), mixing with the rest 2/3 cashmere wool to prepare uniform wool tops, putting into production, and preparing roving through semi-worsted spinning;

s2: producing the fancy yarn PAFA, namely producing fancy yarn on the cashmere roving by adopting a fancy twisting machine to obtain fancy cashmere yarn;

s3: napping, namely napping the finished fancy cashmere yarn;

s4: steaming yarn, namely steaming the napped yarn;

s5: and (5) rewinding, and rewinding the steamed yarns into cone yarns to obtain the finished product.

Comparative example 1:

the preparation of the polymeric hybrid pigment was the same as in example 6.

The silicone oil was prepared as in example 1.

A method for preparing fancy cashmere yarn using colored spun fibers is different from example 1 in that: the pigment used in the dyeing process of step S1 was that of this comparative example.

Test example 1:

1. transmission Electron Microscopy (TEM) test

The JSM-1200EXT20 type transmission electron microscope is adopted to observe the appearance change condition of the pigment red 170 before and after modification, and the accelerating voltage is 80 kV.

The results of the above tests on pigment Red 170 and the polymeric hybrid pigment from example 1 are shown in FIGS. 1 and 2. The analysis in the figure shows that the pigment red 170 has uniform particle size distribution and smooth pigment surface; the surface of the polymer hybrid pigment prepared in example 1 became hazy and had a distinct polymer attachment similar to a glue, indicating that the polymer was effectively coated on the surface of the pigment particles.

2. Infrared Spectroscopy (FTIR) characterization

And testing by using a Spectrum One Fourier transform infrared spectrometer to obtain an infrared Spectrum of the synthesized product, and analyzing each structural group on the Spectrum. Wherein the test wave number range is 4000-500 cm-1And a sweep frequency 32.

The silicone oils obtained in examples 1 and 5 were subjected to the above-described tests, and the results are shown in FIG. 3. As can be seen from the analysis in the figure, the infrared spectra of the two substances are 2160cm-1The characteristic absorption peak of nearby Si-H disappears at 1094cm-1、1014cm-1The vicinity is a characteristic absorption peak of Si-O-Si. In addition, compared with the infrared spectrum of the organic silicon oil prepared in the example 1, the infrared spectrum of the organic silicon oil prepared in the example 5 is 3000-2800 cm-1The characteristic absorption peak intensity of methyl appearing in the range is obviously enhanced and is 1600-1500 cm-1A benzene ring skeleton vibration characteristic absorption peak appears in the range; and at 1250cm-1The intensity of a characteristic absorption peak with ether bonds nearby is obviously enhanced; the above results show that the silicone oil was successfully prepared in example 5.

3. Pigment coating rate test

Centrifuging the prepared sample emulsion, collecting blank latex of supernatant, drying, and weighing and recording as M; weighing and recording m after drying the lower-layer precipitate, and calculating the coating rate according to the following formula:

coating rate is M/(M + M). times.100%

The results of the above tests on the polymer hybrid pigments prepared in comparative example 1 and examples 1-4 are shown in Table 1:

TABLE 1 coating Rate test results

Sample (I) Coating rate/%
Comparative example 1 47.4
Example 1 60.3
Example 2 59.4
Example 3 58.9
Example 4 59.8

From the analysis in table 1, it can be seen that the coating rate of the polymeric hybrid pigment prepared in example 1 is significantly higher than that of comparative example 1, and the presence of 4- [ (2R) -3, 4-dihydro-7-hydroxy-2H-1-benzopyran-2-yl ] -3- (3-methyl-2-buten-1-yl) -1, 2-benzenediol in the polymer monomer can effectively enhance the coating effect of the polymeric hybrid pigment, so that the pigment and the polymer have higher conformity.

4. Dispersion stability test

Taking a polymer hybrid pigment sample, centrifuging for 8min at the rotating speed of 1000r/min, repeating the operation for three times, and drying; then 0.05g of the dried sample is taken and dispersed into 200g of deionized water, and the mixture is uniformly stirred for standby. Ultrasonic stability: and placing the dispersion liquid in a beaker, performing ultrasonic treatment under the power of 150W by using an ultrasonic cell crusher, and sampling and observing the ultraviolet absorption spectrum of the sample for 1min, 15min, 30min and 60min respectively.

The results of the above tests on the polymeric hybrid pigments obtained in comparative example 1 and example 1 are shown in FIGS. 4 and 5. As can be seen from the analysis in the figure, the absorption value of the polymer hybrid pigment prepared in example 1 shown in figure 5 at the maximum absorption wavelength (570nm) is kept unchanged and is obviously increased compared with the absorption value of the polymer hybrid pigment prepared in comparative example 1 shown in figure 4 at the maximum absorption wavelength under different ultrasonic time, which shows that the existence of 4- [ (2R) -3, 4-dihydro-7-hydroxy-2H-1-benzopyran-2-yl ] -3- (3-methyl-2-butene-1-yl) -1, 2-benzenediol in the polymer monomer enables the coated hybrid pigment to keep better dispersion stability under the action of ultrasonic.

5. Storage stability test

The prepared polymer hybrid pigment sample is stored at room temperature, a proper amount of sample is taken every week to test the particle size, and the continuous observation is carried out for 5 weeks.

The results of the above tests on the polymeric hybrid pigments obtained in comparative example 1 and example 1 are shown in FIG. 6. As can be seen from the analysis in the figure, the particle size of the polymeric hybrid pigment obtained in comparative example 1 was increased by 87nm from the initial average particle size, whereas the particle size of the polymeric hybrid pigment of example 1 was increased by only 38nm from the initial average particle size, indicating that the presence of 4- [ (2R) -3, 4-dihydro-7-hydroxy-2H-1-benzopyran-2-yl ] -3- (3-methyl-2-buten-1-yl) -1, 2-benzenediol in the polymer monomer significantly enhanced the storage stability of the polymeric hybrid pigment after being left for 6 weeks.

Test example 2:

cashmere yarn Performance test

The color fastness to light refers to the artificial color fastness of a textile color fastness test of GB/T8427-2008: xenon arc, the rubbing color fastness is tested according to GB/T3920-.

The results of the above tests on the spun-dyed yarns obtained in comparative example 1 and examples 1 to 6 are shown in Table 2:

TABLE 2 dyeing Property test results

As can be seen from the analysis in Table 2, the light fastness, rubbing fastness and washing fastness of the colored spun yarn prepared in example 1 are significantly higher than those of comparative example 1, which shows that the addition of 4- [ (2R) -3, 4-dihydro-7-hydroxy-2H-1-benzopyran-2-yl ] -3- (3-methyl-2-butene-1-yl) -1, 2-benzenediol in the polymer hybrid pigment for dyeing wool can effectively improve the color fastness of dyed fabric, and the grades of the light fastness, rubbing fastness and washing fastness are remarkably improved. The light fastness and the fastness to washing and fading of the prepared colored spun yarn in the embodiment 5 are better than those in the embodiment 1, and the effect of the embodiment 6 is better than that in the comparative example 1, which shows that the light fastness and the fastness to washing and fading of the dyed fabric can be further enhanced by adding the carveol in the organic silicone oil for soft finishing after dyeing of the cashmere wool and compounding with other components.

Apparent color depth K/S value test

The K/S value of the dyed fabric was determined using a CE 7000A color measuring and matching machine.

The results of the above tests on the spun-dyed yarns obtained in comparative example 1 and examples 1 to 6 are shown in Table 3:

TABLE 3K/S value test results

Sample (I) K/S value
Comparative example 1 4.589
Example 1 8.436
Example 2 8.175
Example 3 8.291
Example 4 8.093
Example 5 8.474
Example 6 4.697

As can be seen from the analysis in Table 3, the K/S value of the spun-dyed yarn obtained in example 1 is significantly higher than that of comparative example 1, indicating that the addition of 4- [ (2R) -3, 4-dihydro-7-hydroxy-2H-1-benzopyran-2-yl ] -3- (3-methyl-2-buten-1-yl) -1, 2-benzenediol to the polymer hybrid pigment for dyeing of cashmere wool is effective in enhancing the dye uptake of the pigment. The K/S value of the resultant spun-dyed yarn of example 5 was comparable to that of example 1, and the effect of example 6 was comparable to that of comparative example 1, indicating that the addition of carveol to the soft-finish silicone oil after dyeing of the cashmere wool did not negatively affect the dye uptake of the pigment on the fabric.

Tensile Properties

The test is carried out according to GB/T3916-2013 CRE method for determining the breaking strength and the breaking elongation of single yarn of the textile reeled yarn.

The results of the above tests on the spun-dyed yarns obtained in comparative example 1 and examples 1 to 6 are shown in Table 4:

TABLE 4 mechanical Property test results

Sample (I) Breaking strength (cN/tex) Elongation at Break (%)
Comparative example 1 0.95 8.42
Example 1 1.36 8.94
Example 2 1.21 8.67
Example 3 1.25 8.75
Example 4 1.20 8.49
Example 5 2.03 15.18
Example 6 1.57 14.73

As can be seen from the analysis in Table 3, the breaking strength of the spun-dyed yarn obtained in example 1 is significantly higher than that of comparative example 1, indicating that the addition of 4- [ (2R) -3, 4-dihydro-7-hydroxy-2H-1-benzopyran-2-yl ] -3- (3-methyl-2-buten-1-yl) -1, 2-benzenediol to the polymer hybrid pigment for dyeing cashmere wool can effectively enhance the breaking strength of the spun-dyed yarn and improve the mechanical properties thereof. The breaking strength and the breaking elongation of the colored spun yarn prepared in the embodiment 5 are better than those of the embodiment 1, the effect of the embodiment 6 is better than that of the comparative example 1, and the result shows that the mechanical property of the colored spun yarn can be effectively enhanced by adding the carveol in the organic silicone oil for soft finishing after dyeing the cashmere wool and compounding with other components.

Test example 3:

testing of the Properties of the dyed, Soft finished fibers

Test for Friction Properties

Testing an instrument: the coefficient of friction tester, model Y151, was purchased from second textile machinery, Inc., Changzhou. And (3) testing conditions are as follows: under the standard atmospheric condition, the pre-tension is 100mg, when the static friction coefficient is measured, the handle position is BCG, and the rotating speed is 1 r/min; when the sliding friction coefficient is measured, the position of the handle is ADG, and the rotating speed is 30 r/min. Calculating the friction coefficient according to the euler formula:

in the formula, f is the weight of the fiber food hanging tension clamp, 100 mg; f. of0The difference between the mass of the suspended tension tong and the reading m of the torsion balance is in mg; μ -coefficient of friction between rope and cylindrical surface; theta-the contact angle of the string with the cylindrical surface.

The friction coefficient between fibers can be used for representing the spinnability of the fibers, and the smaller the value of Delta mu-static-mu movement is, the fibers have smooth hand feeling, and the fibers are easier to be carded and drafted in the spinning process.

The dyed, soft-finished fibers from examples 1 and 5 were tested as described above and the results are shown in table 5:

TABLE 5 Friction Performance test results

Sample (I) △μ
Example 1 0.0769
Example 5 0.0345

The value of delta mu of the dyed and soft-finished fiber prepared in the embodiment 5 is lower than that of the embodiment 1, which shows that the surface performance of the fiber can be effectively improved and the smoothness of the cashmere fiber can be enhanced by adding the carveol in the organic silicone oil for soft finishing after dyeing cashmere wool and compounding with other components.

Conventional techniques in the above embodiments are known to those skilled in the art, and therefore, will not be described in detail herein.

The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.

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