CN1465758A - Method for preparing colorant used in producing color acrylic fibre by mass coloration method - Google Patents
Method for preparing colorant used in producing color acrylic fibre by mass coloration method Download PDFInfo
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- CN1465758A CN1465758A CNA02112308XA CN02112308A CN1465758A CN 1465758 A CN1465758 A CN 1465758A CN A02112308X A CNA02112308X A CN A02112308XA CN 02112308 A CN02112308 A CN 02112308A CN 1465758 A CN1465758 A CN 1465758A
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- pigment
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Abstract
The present invention relates to a preparation method of coloring material for producing colored acrylic fiber by adopting mass coloration process. Said method includes the following steps: mixing pigment, dispersing agent and NaSCN aqueous solution and grinding in ball-grinding machine, in the coloring material the pigment content is 5-25 wt%, the weight ratio of pigment and dispersing agent is 100:3-30, and the ginding time is 0.5-5.0, then the coloring material product can be obtained. The above-mentioned dispersing agent is one compound selected from naphthalenesulfonate formaldehyde condensate, methyl naphthalene sulfonate formaldehyde condensate or benzyl naphthalene sulfonate formaldehyde condensate or mixture of them, and the pigment is carbon black, phthalocyanine blue, iron oxide or ultrasmarine.
Description
Technical field
The present invention relates to the preparation of colorant used in mass coloration of acrylic fibre spinning, particularly adopt the preparation method of NaSCN wet spinning technology original liquid coloring manufactured color acrylic fibre with colouring agent.
Background technology
Original liquid coloring is made the new technology that color acrylic fibre is chemical fibre industry generation in modern age before spinning, and its development is very fast, and has obtained using than extensive industrialized.The development of acrylic fibers original liquid coloring spining technology is so rapid, and its main cause is to have plurality of advantages such as the dyeing cost is low, the gained fiber colour is even, COLOR FASTNESS is high, color matching is convenient compared with traditional fiber, yarn dyeing technology.Yet what is more important since painted be in fiber production process, to carry out, can as dyeing in traditional dyeing and finishing technology and rinsing process, not produce a large amount of sewage, with regard to the protection of environment and water resource, its advantage is fairly obvious.
Original liquid coloring manufactured color acrylic fibre generally is that required colouring agent is prepared by spinning factory when stoste prepares, then itself and spinning solution are hybridly prepared into coloured spinning solution, send the spinning machine spinning, introduce as patent DE 78-2823169, DD 224043 A1, DD259203 A1, JP 03104916 A2 and JP 03104917 A2.This method is that the replacing color is very difficult for the maximum problem of spinning factory, because will produce a large amount of transition material in case change color, waste is serious.Obviously once preparing a large amount of colouring agents is best solution, yet can stably store be very crucial to colouring agent.In existing original liquid coloring manufactured color acrylic fibre technology, colouring agent can't be stablized preservation usually for a long time, and pigment cohesion caking is a common phenomena, and the weight meta particle diameter of granules of pigments is 1 μ m in the general colouring agent.
Summary of the invention
Technical problem to be solved by this invention provides a kind of preparation method of colorant used in mass coloration of acrylic fibre spinning, the colouring agent for preparing gained with this method can be stablized preservation for a long time, pigment does not have the cohesion caking phenomenon, to overcome the existing in prior technology defective.
Below be the technical scheme that the present invention solves the problems of the technologies described above:
A kind of preparation method who is used for the colouring agent of producing color acrylic fibre by mass coloration, this method comprises and will grind in ball mill after pigment, dispersant and the NaSCN aqueous solution, in colouring agent, the content of pigment is 5～25wt%, the weight ratio of pigment and dispersant is 100: 3～30, grind and obtain the colouring agent product after 0.5～5.0 hour, above-mentioned dispersant is taken from a kind of compound in naphthalenesulfonate formaldehyde condensation compound, methyl naphthalene sulfonic acid salt formaldehyde condensation products or the benzyl naphthalenesulfonate formaldehyde condensation compound or the mixture of two or more compounds.
The weight ratio of above-mentioned pigment and dispersant is preferably 100: 5～and 20; The concentration of the described NaSCN aqueous solution can be 40～60wt%; The rotating speed of ball mill generally should be controlled to be 100～250 rev/mins during grinding.And pigment is generally carbon black, phthalocyanine blue, iron oxide or ultramarine.
For the present invention, the inventor thinks the definite relatively more crucial of the selection of dispersant and addition.In pigment and process that NaSCN solution mixes, pass through pulverizing, dispersion and stabilisation three phases, selected dispersant has all played positive effect to above three processes among the present invention.In the initial period of pigment grind, dispersant be added with the disaggregation that helps the pigment particles aggregate body, dispersant is dispersed in the NaSCN solution system granules of pigments by sterically hindered effect and ionic charge repulsion after the fragmentation of pigment aggregation, and stabilisation subsequently is more important, and the dispersion effect of dispersant more is embodied on the stability of grinding back granules of pigments dispersion.No matter from the angle of preparation or the angle of use, the content of pigment in painted is unsuitable too high, is more satisfactory in 5～25% scope usually.The addition of dispersant is determined according to the amount of pigment that then the inventor thinks that the weight ratio of pigment and dispersant generally should be controlled at 100: 3～30, and surpassing 100: 30 back dispersing of pigments does not have tangible raising.
The colouring agent of preparation gained did not have tangible lamination and coacervation later at least 30 days in placement, and demonstrating the carbon black dispersion cording has good dispersion stabilization, and the weight meta particle diameter of granules of pigments can maintain 0.4～0.7 μ m in the general colouring agent.After the colouring agent for preparing adds in the polyacrylonitrile spinning solution, very little to the influence of polyacrylonitrile stoste spinning process middle filtrator spare.This shows that compared with prior art good effect of the present invention is very tangible.
The specific embodiment [embodiment 1]
Fully mixing is stirred with the 51.7wt%NaSCN solution of the dispersant naphthalenesulfonate formaldehyde condensation compound aequum of aequum by elder generation in ball mill, add the pigment carbon black of aequum then, continues to be stirred to abundant mixing.Wherein, the content of pigment carbon black is 8wt%, and the weight ratio of pigment and dispersant is 100: 5.Mix the back start that finishes and grind, drum's speed of rotation is controlled to be 200 rev/mins, and milling time is 2.0 hours.By analysis, the weight meta particle diameter of granules of pigments is 0.47 (μ m) in the product; The weight ratio surface area is 8.5160 (m
2/ g).
The colouring agent that makes was placed after 50 days, reanalysed product, and the result is as follows:
Weight meta particle diameter: 0.49 (μ m); Weight ratio surface area: 7.7857 (m
2/ g).[embodiment 2]
Fully mixing is stirred with the 51.7wt%NaSCN solution of the dispersant methyl naphthalene sulfonic acid salt formaldehyde condensation products aequum of aequum by elder generation in ball mill, add the pigment carbon black of aequum then, continues to be stirred to abundant mixing.Wherein, the content of pigment carbon black is 12wt%, and the weight ratio of pigment and dispersant is 100: 10.Mix the back start that finishes and grind, drum's speed of rotation is controlled to be 200 rev/mins, and milling time is 1.0 hours.By analysis, the weight meta particle diameter of granules of pigments is 0.44 (μ m) in the product; The weight ratio surface area is 8.7967 (m
2/ g).
The colouring agent that makes was placed after 50 days, reanalysed product, and the result is as follows:
Weight meta particle diameter: 0.46 (μ m); Weight ratio surface area: 7.7857 (m
2/ g).[embodiment 3]
Fully mixing is stirred with the 51.7wt%NaSCN solution of the dispersant benzyl naphthalenesulfonate formaldehyde condensation compound aequum of aequum by elder generation in ball mill, add the pigment carbon black of aequum then, continues to be stirred to abundant mixing.Wherein, the content of pigment carbon black is 25wt%, and the weight ratio of pigment and dispersant is 100: 20.Mix the back start that finishes and grind, drum's speed of rotation is controlled to be 200 rev/mins, and milling time is 3.0 hours.By analysis, the weight meta particle diameter of granules of pigments is 0.52 (μ m) in the product; The weight ratio surface area is 6.0250 (m
2/ g).
The colouring agent that makes was placed after 50 days, reanalysed product, and the result is as follows:
Weight meta particle diameter: 0.56 (μ m); Weight ratio surface area: 5.4216 (m
2/ g).[embodiment 4]
Fully mixing is stirred with the 51.7wt%NaSCN solution of the dispersant naphthalenesulfonate formaldehyde condensation compound aequum of aequum by elder generation in ball mill, add the pigment phthalocyanine blue of aequum then, continues to be stirred to abundant mixing.Wherein, the content of pigment phthalocyanine blue is 25wt%, and the weight ratio of pigment and dispersant is 100: 30.Mix the back start that finishes and grind, drum's speed of rotation is controlled to be 200 rev/mins, and milling time is 5 hours.By analysis, the weight meta particle diameter of granules of pigments is 0.49 (μ m) in the product; The weight ratio surface area is 8.7642 (m
2/ g).
The colouring agent that makes was placed after 50 days, reanalysed product, and the result is as follows:
Weight meta particle diameter: 0.52 (μ m); Weight ratio surface area: 7.5538 (m
2/ g).[embodiment 5]
Fully mixing is stirred with the 51.7wt%NaSCN solution of the dispersant methyl naphthalene sulfonic acid salt formaldehyde condensation products aequum of aequum by elder generation in ball mill, add the pigment phthalocyanine blue of aequum then, continues to be stirred to abundant mixing.Wherein, the content of pigment phthalocyanine blue is 12wt%, and the weight ratio of pigment and dispersant is 100: 15.Mix the back start that finishes and grind, drum's speed of rotation is controlled to be 200 rev/mins, and milling time is 2.5 hours.By analysis, the weight meta particle diameter of granules of pigments is 0.57 (μ m) in the product; The weight ratio surface area is 6.7976 (m
2/ g).
The colouring agent that makes was placed after 50 days, reanalysed product, and the result is as follows:
Weight meta particle diameter: 0.62 (μ m); Weight ratio surface area: 5.0359 (m
2/ g).[embodiment 6]
Fully mixing is stirred with the 51.7wt%NaSCN solution of the dispersant benzyl naphthalenesulfonate formaldehyde condensation compound aequum of aequum by elder generation in ball mill, add the pigment ultramarine of aequum then, continues to be stirred to abundant mixing.Wherein, the content of pigment ultramarine is 5wt%, and the weight ratio of pigment and dispersant is 100: 5.Mix the back start that finishes and grind, drum's speed of rotation is controlled to be 200 rev/mins, and milling time is 3 hours.By analysis, the weight meta particle diameter of granules of pigments is 0.48 (μ m) in the product; The weight ratio surface area is 8.9754 (m
2/ g).
The colouring agent that makes was placed after 50 days, reanalysed product, and the result is as follows:
Weight meta particle diameter: 0.52 (μ m); Weight ratio surface area: 7.6138 (m
2/ g).[embodiment 7]
Fully mixing is stirred with the 51.7wt%NaSCN solution of the dispersant naphthalenesulfonate formaldehyde condensation compound aequum of aequum by elder generation in ball mill, add the pigment ultramarine of aequum then, continues to be stirred to abundant mixing.Wherein, the content of pigment ultramarine is 25wt%, and the weight ratio of pigment and dispersant is 100: 10.Mix the back start that finishes and grind, drum's speed of rotation is controlled to be 200 rev/mins, and milling time is 5.0 hours.By analysis, the weight meta particle diameter of granules of pigments is 0.68 (μ m) in the product; The weight ratio surface area is 5.0286 (m
2/ g).
The colouring agent that makes was placed after 50 days, reanalysed product, and the result is as follows:
Weight meta particle diameter: 0.73 (μ m); Weight ratio surface area: 5.1628 (m
2/ g).[embodiment 8]
Fully mixing is stirred with the 51.7wt%NaSCN solution of the dispersant methyl naphthalene sulfonic acid salt formaldehyde condensation products aequum of aequum by elder generation in ball mill, add the pigment iron oxide of aequum then, continues to be stirred to abundant mixing.Wherein, the content of pigment iron oxide is 8wt%, and the weight ratio of pigment and dispersant is 100: 20.Mix the back start that finishes and grind, drum's speed of rotation is controlled to be 200 rev/mins, and milling time is 4.0 hours.By analysis, the weight meta particle diameter of granules of pigments is 0.54 (μ m) in the product; The weight ratio surface area is 7.8963 (m
2/ g).
The colouring agent that makes was placed after 50 days, reanalysed product, and the result is as follows:
Weight meta particle diameter: 0.59 (μ m); Weight ratio surface area: 6.4475 (m
2/ g).[embodiment 10]
Fully mixing is stirred with the 51.7wt%NaSCN solution of the dispersant methyl naphthalene sulfonic acid salt formaldehyde condensation products aequum of aequum by elder generation in ball mill, add the pigment phthalocyanine blue of aequum then, continues to be stirred to abundant mixing.Wherein, the content of pigment phthalocyanine blue is 8wt%, and the weight ratio of pigment and dispersant is 100: 20.Mix the back start that finishes and grind, drum's speed of rotation is controlled to be 200 rev/mins, and milling time is 3.0 hours.By analysis, the weight meta particle diameter of granules of pigments is 0.44 (μ m) in the product; The weight ratio surface area is 8.8238 (m
2/ g).
The colouring agent that makes was placed after 50 days, reanalysed product, and the result is as follows:
Weight meta particle diameter: 0.46 (μ m); Weight ratio surface area: 8.8564 (m
2/ g).
Claims (5)
1, a kind of preparation method who is used for the colouring agent of producing color acrylic fibre by mass coloration, this method comprises and will grind in ball mill after pigment, dispersant and the NaSCN aqueous solution, in colouring agent, the content of pigment is 5～25wt%, the weight ratio of pigment and dispersant is 100: 3～30, grind and obtain the colouring agent product after 0.5～5.0 hour, above-mentioned dispersant is taken from a kind of compound in naphthalenesulfonate formaldehyde condensation compound, methyl naphthalene sulfonic acid salt formaldehyde condensation products or the benzyl naphthalenesulfonate formaldehyde condensation compound or the mixture of two or more compounds.
2, the preparation method who is used for the colouring agent of producing color acrylic fibre by mass coloration according to claim 1, the weight ratio that it is characterized in that described pigment and dispersant is 100: 5～20.
3, the preparation method who is used for the colouring agent of producing color acrylic fibre by mass coloration according to claim 1, the concentration that it is characterized in that the described NaSCN aqueous solution is 40～60wt%.
4, the preparation method who is used for the colouring agent of producing color acrylic fibre by mass coloration according to claim 1 is characterized in that the rotating speed of described ball mill is controlled to be 100～250 rev/mins.
5,, it is characterized in that described pigment is carbon black, phthalocyanine blue, iron oxide or ultramarine according to claim 1,2, the 3 or 4 described preparation methods that are used for the colouring agent of producing color acrylic fibre by mass coloration.
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| Application Number | Priority Date | Filing Date | Title |
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| CNA02112308XA CN1465758A (en) | 2002-06-28 | 2002-06-28 | Method for preparing colorant used in producing color acrylic fibre by mass coloration method |
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| CNA02112308XA CN1465758A (en) | 2002-06-28 | 2002-06-28 | Method for preparing colorant used in producing color acrylic fibre by mass coloration method |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1329456C (en) * | 2004-10-15 | 2007-08-01 | 东港工贸集团有限公司 | Alkali proof stabilizer for active dye |
| CN103031757A (en) * | 2012-12-28 | 2013-04-10 | 苏州世名科技股份有限公司 | Black water-based color paste for acrylic stock solution coloring and preparation method of black water-based color paste |
| CN105369385A (en) * | 2014-08-26 | 2016-03-02 | 中国石油化工股份有限公司 | Stock solution coloring acrylic fibers having high color fastness and preparation method |
| CN105463601A (en) * | 2014-08-26 | 2016-04-06 | 中国石油化工股份有限公司 | Acrylic pigment slurry, preparation method and application thereof |
-
2002
- 2002-06-28 CN CNA02112308XA patent/CN1465758A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1329456C (en) * | 2004-10-15 | 2007-08-01 | 东港工贸集团有限公司 | Alkali proof stabilizer for active dye |
| CN103031757A (en) * | 2012-12-28 | 2013-04-10 | 苏州世名科技股份有限公司 | Black water-based color paste for acrylic stock solution coloring and preparation method of black water-based color paste |
| CN105369385A (en) * | 2014-08-26 | 2016-03-02 | 中国石油化工股份有限公司 | Stock solution coloring acrylic fibers having high color fastness and preparation method |
| CN105463601A (en) * | 2014-08-26 | 2016-04-06 | 中国石油化工股份有限公司 | Acrylic pigment slurry, preparation method and application thereof |
| CN105369385B (en) * | 2014-08-26 | 2019-08-13 | 中国石油化工股份有限公司 | A kind of Dope Dyed Acrylic Fiber and preparation method with high color fastness |
| CN105463601B (en) * | 2014-08-26 | 2019-08-13 | 中国石油化工股份有限公司 | A kind of acrylic fibers dispersible pigment color paste, preparation method and applications |
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