CN103789858B - A kind of environment-friendly type thermostable durable flame-retardant fiber and preparation method thereof - Google Patents

A kind of environment-friendly type thermostable durable flame-retardant fiber and preparation method thereof Download PDF

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CN103789858B
CN103789858B CN201410039251.0A CN201410039251A CN103789858B CN 103789858 B CN103789858 B CN 103789858B CN 201410039251 A CN201410039251 A CN 201410039251A CN 103789858 B CN103789858 B CN 103789858B
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retardant
glue
spinning
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CN103789858A (en
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刘承修
毕慎平
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The blue fire resistance fibre of Beijing Sail Co., Ltd
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刘承修
毕慎平
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Abstract

The invention discloses a kind of environment-friendly type thermostable durable flame-retardant fiber and preparation method thereof, the raw material of described environment-friendly type thermostable durable flame-retardant fiber comprises cellulose, fire retardant and cationic cross linking agent, described fire retardant is silicon nitrogenated flame retardant, and its feature of environmental protection, anti-flammability meet state related requirements.Apply preparation method of the present invention, the spinning that silicon based flame retardant in the past easily causes viscose glue age gelation to cause can be overcome and pause, because intensity is low and flame-retardant composition is lost the downstream of causing and spinned, weaves difficulty and take the lasting flame retardant effect in process.The long filament of this explained hereafter and short silk are available for pin, the textiles that making clothes, household, army's protection and public decoration use.

Description

A kind of environment-friendly type thermostable durable flame-retardant fiber and preparation method thereof
Technical field
The invention belongs to chemical fibre manufacture field, particularly a kind of environment-friendly type thermostable durable flame-retardant fiber and preparation method thereof.
Background technology
Fire-retardant science and technology is that the mankind are in order to adapt to the needs of social development; prevention and corntrol fire; protection human life's property safety and a science growing up, be occur for fire and the rule of development, the principle of substance combustion, and take the scientific method suppressing burning.Flame-retarded technology, according to the combustion characteristics of combustible material, makes it be converted into flame retardancy or non-automatic incombustible material, reduces the speed of substance combustion, stops fire to expand.
Along with the development of social material civilization, flame-retarded technology is subject to the great attention of people day by day, just utilizes alum, borax, ferrous sulfate mixture to make cellulose fabric and paper pulp etc. fire-retardant as far back as Englishman in 1785.Within 1913, dyestuff scientist moors gold on the basis of previous work, proposes durable fabrics flame resistance process theory.After the sixties, along with the formulation of many National Fire regulations, flame-retarded technology has had on the textile to be applied more widely, but relate generally to the surface flame-retardant process of fabric or use halogen and phosphorus series organic compound fire retardant, as Lenging(Austria), Polynosic(Japan) HFG(Japan), these are containing the fiber of organic compound flame retardant, although flame retardant effect is better, but to environment unfriendly or burning time can discharge a large amount of poison gas and smog, there is safety and environmental problem.What have positive effect is Visil(Finland) and Anti-fell(Shandong) fiber, with inorganic polysilicon acid or its salt for flame-retardant composition.(the patent No.: ZL94110065.0 that Chinese patent has " flame-retarding fibre of cellulose polysilicate and production method thereof "; Patentee: Zhao Yushan, Feng Shouzhi, Wang Huifu; The applying date: on February 3rd, 1994); " preparation method of regenerated cellulose/nanosized SiO_2 flame-proof composite material " (patent No.: 20051004231409; Patentee: University Of Qingdao; The applying date: on January 7th, 2005).
But above-mentioned salt based flame retardant is not wrapped by, very easily cause the accelerated ageing of viscose glue stoste, viscosity increases severely, cannot spinning because of gelation, maybe can not be formed effectively fixing, fiber Final finishing, dye, weave and knitted fabric and textile use procedure in lose flame retardant effect; On the other hand, because adding of these fire retardants causes viscose fiber strength to reduce, cause downstream and spin, weave, take difficulty and cannot industrialization be realized always.In sum, a kind of fire retardant that can suppress salting-out effect is badly in need of at present.
Summary of the invention
The object of this invention is to provide a kind of environment-friendly type thermostable durable flame-retardant fiber and preparation method thereof.Wherein, what be different from above-mentioned technology or patent is the use of a kind of fire retardant that can suppress salting-out effect, adds behind IIIF position, ensure that fire retardant at the time inner gel of spinning technique requirement, can not avoid scrap rubber simultaneously and produce after mixing with viscose glue; At finishing process by adding cationic cross linking agent, make the flame retardant constituent in fiber form netted soluble thing, flame-retardant composition is not easily lost, and substitutes caustic wash desulfuration simultaneously, simplifies operation; Carrying out 2 ~ 3 drawing-offs to initial set strand makes fibre strength increase, and then realizes serialization, large-scale production.
The object of the invention is to be achieved through the following technical solutions:
A kind of environment-friendly type thermostable durable flame-retardant fiber, the raw material of described fire resistance fibre comprises cellulose, fire retardant, cationic cross linking agent, and the weight fraction ratio of each raw material described is:
Cellulose 65 ~ 84
Fire retardant 16 ~ 35
Cationic cross linking agent 1 ~ 3.
Further, the described cellulosic degree of polymerization is 600 ~ 800.
Further, the ionic species of described cationic cross linking agent is Ti 4+, RN 3+, Al 3+, Ca 2+the mixture of one or more.
Another object of the present invention is achieved through the following technical solutions:
A preparation method for environment-friendly type thermostable durable flame-retardant fiber, said method comprising the steps of:
1) preparation of viscose glue stoste is by traditional viscose glue stoste preparation method, by cellulose through the operation such as alkali lye Jin Ze, squeezing, pulverizing, experienced, sulfonation, together filtration, two road filtrations, three road filtrations, deaeration, is prepared into spinning veiscose stoste, i.e. IIIF glue;
2) preparation of Retardant Injection liquid is according to dispersant: 10% alkali lye: fire retardant=(0.05 ~ 0.0769): (0.2 ~ 0.23): the volume ratio of (0.59 ~ 0.69) is allocated, and the Retardant Injection liquid prepared remains in stirring;
3) fire retardant spin before injection by step 1), step 2) the IIIF glue for preparing and the mixing of Retardant Injection liquid, described IIIF glue and Retardant Injection liquid volume ratio are:
IIIF glue 69 ~ 79
Retardant Injection liquid 31 ~ 21;
By dynamic and static state blender before described Retardant Injection liquid injection spinning head, after mixing, obtain anti-flaming viscose;
4) anti-flaming viscose obtained in step 3) is sprayed by spinning head and obtains spinning by spinning, and described spinning obtains fire resistance fibre head product through acid bath, and wherein, shower nozzle aperture is 0.045 ~ 0.065mm, shower nozzle drawing-off 50 ~ 60%, plasticizing drawing-off 50 ~ 100%;
5) concise described fire resistance fibre head product is respectively through washing together, two road washings, and solidification desulfurization, three roads are washed, oiled, and namely obtain described environment-friendly type thermostable durable flame-retardant fiber;
Further, consisting of of the IIIF glue in described step 1:
First fibre 8.1 ~ 9.8%
NaOH 5.4 ~ 7.8%;
The viscosity of described IIIF glue 40 ~ 60 seconds, degree of ripeness 14 ~ 16ml(10% ammonium chloride).
Further, dispersant described in described step 2 is polyvinyl alcohol, and described alkali lye is sodium hydroxide solution.
Further, in described step 3, the addition manner of fire retardant is for spinning front injection, and before adopting injector or compressed air that Retardant Injection liquid is injected spinning head, dynamic and static state blender mixes glue, consisting of of described anti-flaming viscose:
First fibre 9 ~ 9.5%
Alkali 7.8 ~ 8.1%;
The viscosity >27S of described anti-flaming viscose, degree of ripeness (15%NH 4cl) 8 ~ 9ml.
Further, the raw material in the acid bath solution in described step 4 comprises sulfuric acid, sodium sulphate, zinc sulfate, and the weight fraction ratio of each raw material described is:
Sulfuric acid 70 ~ 145
Sodium sulphate 220 ~ 350
Zinc sulfate 14 ~ 90;
Described acid bath temperature is 36 DEG C ~ 55 DEG C.
Further, solidify in desulfurization described in described step 5, the raw material of body lotion used comprises soft water, cationic cross linking agent and sodium hydrogensulfite, and the weight fraction ratio of each raw material described is:
Soft water 0.66
Cationic cross linking agent 0.33
Sodium hydrogensulfite 0.01;
The temperature of solidifying desulfurization described in described step 5 is 75 ~ 90 DEG C, and the time is 8 ~ 15 minutes.
Another object of the present invention is achieved through the following technical solutions:
An application for environment-friendly type thermostable durable flame-retardant fiber, described fire resistance fibre, for making knitwear, is preferred for clothes, household, military project shielding and public decoration.
the present invention's beneficial effect is compared with prior art:
1, fire resistance fibre of the present invention shaping after, dry fracture strength >=1.85cn/dtex, moisture 8% ~ 15%, still fiber shape can be maintained under 1200 DEG C of aerobic conditions, without melting dropping under hot conditions, silk fabrics can form shielding protection layer, limited oxygen index LOI >=28%;
2, the preparation method of fire resistance fibre of the present invention compared to existing technology, more simplify by technique, reduced caustic wash desulfuration operation, reduced processing cost, more environmental protection;
3, fire resistance fibre of the present invention, structure is the large molecule of crossover network, can adapt to acid, alkali and various complicated, and the intensity of described fire resistance fibre is high, high temperature resistant, wash resistant, is suitable for the manufacture of pin, textiles.
Detailed description of the invention
embodiment 1
A kind of environment-friendly type thermostable durable flame-retardant fiber, the raw material of described fire resistance fibre comprises cellulose, fire retardant, cationic cross linking agent, and the weight fraction ratio of each raw material described is:
Cellulose 65 ~ 84
Fire retardant 16 ~ 35
Cationic cross linking agent 1 ~ 3.
Further, the described cellulosic degree of polymerization is 600 ~ 800.
Further, described fire retardant is silica nitrogen heterocyclic compounds.
Further, the ionic species of described cationic cross linking agent is Ti 4+, RN 3+, Al 3+, Ca 2+the mixture of one or more.
Another object of the present invention is achieved through the following technical solutions:
A preparation method for environment-friendly type thermostable durable flame-retardant fiber, said method comprising the steps of:
1) preparation of viscose glue stoste is by traditional viscose glue stoste preparation method, by cellulose through the operation such as alkali lye Jin Ze, squeezing, pulverizing, experienced, sulfonation, together filtration, two road filtrations, three road filtrations, deaeration, is prepared into spinning veiscose stoste, i.e. IIIF glue;
2) preparation of Retardant Injection liquid is according to dispersant: 10% alkali lye: fire retardant=(0.05 ~ 0.0769): (0.2 ~ 0.23): the volume ratio of (0.59 ~ 0.69) is allocated, and the Retardant Injection liquid prepared remains in stirring;
3) fire retardant spin before injection by step 1), step 2) the IIIF glue for preparing and the mixing of Retardant Injection liquid, described IIIF glue and Retardant Injection liquid volume ratio are:
IIIF glue 69 ~ 79
Retardant Injection liquid 31 ~ 21;
By dynamic and static state blender before described Retardant Injection liquid injection spinning head, after mixing, obtain anti-flaming viscose;
4) anti-flaming viscose obtained in step 3) is sprayed by spinning head and obtains spinning by spinning, and described spinning obtains fire resistance fibre head product through acid bath, and wherein, shower nozzle aperture is 0.045 ~ 0.065mm, shower nozzle drawing-off 50 ~ 60%, plasticizing drawing-off 50 ~ 100%;
5) concise described fire resistance fibre head product is respectively through washing together, two road washings, and solidification desulfurization, three roads are washed, oiled, and namely obtain described environment-friendly type thermostable durable flame-retardant fiber;
Further, consisting of of the IIIF glue in described step 1:
First fibre 8.1 ~ 9.8%
NaOH 5.4 ~ 7.8%;
The viscosity of described IIIF glue 40 ~ 60 seconds, degree of ripeness 14 ~ 16ml(10% ammonium chloride).
Further, dispersant described in described step 2 is polyvinyl alcohol, and described alkali lye is sodium hydroxide solution.
Further, in described step 3, the addition manner of fire retardant is for spinning front injection, and before adopting injector or compressed air that Retardant Injection liquid is injected spinning head, dynamic and static state blender mixes glue, consisting of of described anti-flaming viscose:
First fibre 9 ~ 9.5%
Alkali 7.8 ~ 8.1%;
The viscosity >27S of described anti-flaming viscose, degree of ripeness (15%NH 4cl) 8 ~ 9ml.
Further, the raw material in the acid bath solution in described step 4 comprises sulfuric acid, sodium sulphate, zinc sulfate, and the weight fraction ratio of each raw material described is:
Sulfuric acid 70 ~ 145
Sodium sulphate 220 ~ 350
Zinc sulfate 14 ~ 90;
Described acid bath temperature is 36 DEG C ~ 55 DEG C.
Further, solidify in desulfurization described in described step 5, the raw material of body lotion used comprises soft water, cationic cross linking agent and sodium hydrogensulfite, and the weight fraction ratio of each raw material described is:
Soft water 0.66
Cationic cross linking agent 0.33
Sodium hydrogensulfite 0.01;
The temperature of solidifying desulfurization described in described step 5 is 75 ~ 90 DEG C, and the time is 8 ~ 15 minutes.
The present embodiment unit of weight used is kilogram, also can be gram;
Each raw material described in the present embodiment is technical grade;
Each component described in the present embodiment is the conventional products that market is sold, and described fire retardant is the phosphorus system viscose glue combustion inhibitor special DX1212 that silicon nitrogen system viscose glue combustion inhibitor special, the Sandoflame5060 of gram Lay benefactor department production or lucky Su Chemical Co., Ltd. that Xinxiang mayor expands Chemical Co., Ltd. and produces produce.
In the present embodiment, each raw material in described environment-friendly type thermostable durable flame-retardant fiber can in the ratio range provided flexible combination, do not enumerate one by one at this.
embodiment 2
The present embodiment is the preferred version on embodiment 1 basis, and raw materials used quality is identical with embodiment 1, and please refer to embodiment 1 with embodiment 1 same section, the present embodiment said method comprising the steps of:
Making viscose stoste is by traditional viscose glue stoste preparation method, and cotton (wood) cellulose, through the operation such as alkali lye Jin Ze, squeezing, pulverizing, experienced, sulfonation, one filtration, two road filtrations, three road filtrations, deaeration, is prepared into spinning veiscose stoste (IIIF glue).Require consisting of of IIIF glue: first fibre 8.1 ~ 9.8%; NaOH 5.4 ~ 7.8%.Require the viscosity 40 ~ 60 seconds (falling ball method) of IIIF glue; Degree of ripeness 14 ~ 16ml(10% ammonium chloride).The preparation of Retardant Injection liquid is according to dispersant again: 10% alkali lye: fire retardant=(0.05 ~ 0.0769): (0.2 ~ 0.23): the volume ratio of (0.59 ~ 0.69) is allocated, the Retardant Injection liquid prepared remains in stirring.By 180L Retardant Injection liquid, inject 1000LIIIF viscose glue with injector or compressed air, after dynamic and static state blender combined balance system, connect de-obtained spinning glue.At sulfuric acid 110g/L, sodium sulphate 245g/L, zinc sulfate 25g/L, return acid concentration drop and be less than 4.0, spinning in the acid bath of acid temperature 55 DEG C, and shower nozzle specification is 1900(hole) × 0.065mm(aperture).Strand is through secondary drawing-off, and shower nozzle drawing-off 50%, plastifies drawing-off 50%.Cut off, obtained 1.0DX36mm viscose short-thread, fiber, after twice washing, carries out crosslinked fixing, and solidification desulfurization body lotion consists of: soft water: cationic cross linking agent: sodium hydrogensulfite=0.66:0.33:0.01.Solidification desulfurization temperature is 75 ~ 90 DEG C, and the time is 8 ~ 15 minutes.Then wash, dehydration, oils, and dries obtained heat-resistant fireproof viscose short-thread.
The heat-resistant fireproof viscose short-thread obtained, its dry fracture strength >=1.85cn/dtex, moisture 8% ~ 15%; still fiber shape can be maintained under 1200 DEG C of aerobic conditions; without melting dropping under hot conditions, silk fabrics can form shielding protection layer, limited oxygen index LOI >=28%.
embodiment 3
The present embodiment is the preferred version on embodiment 1 basis, and raw materials used quality is identical with embodiment 1, and please refer to embodiment 1 with embodiment 1 same section, the present embodiment said method comprising the steps of:
First Making viscose stoste is by traditional viscose glue stoste preparation method, cotton (wood) cellulose, through the operation such as alkali lye Jin Ze, squeezing, pulverizing, experienced, sulfonation, one filtration, two road filtrations, three road filtrations, deaeration, is prepared into spinning veiscose stoste (IIIF glue).Require consisting of of IIIF glue: first fibre 8.1 ~ 9.8%; NaOH 5.4 ~ 7.8%.Require the viscosity 40 ~ 60 seconds (falling ball method) of IIIF glue; Degree of ripeness 14 ~ 16ml(10% ammonium chloride).The preparation of Retardant Injection liquid is according to dispersant again: 10% alkali lye: fire retardant=(0.05 ~ 0.0769): (0.2 ~ 0.23): the volume ratio of (0.59 ~ 0.69) is allocated, the Retardant Injection liquid prepared remains in stirring.By 180L Retardant Injection liquid, inject 1000LIIIF viscose glue with injector or compressed air, obtained spinning glue after dynamic and static state blender combined balance system.At sulfuric acid 110g/L, sodium sulphate 245g/L, zinc sulfate 25g/L, return acid concentration drop and be less than 2.0, and spinning in the acid bath of acid temperature 55 DEG C, shower nozzle hole count is 24 holes, and bicycle speed is 73m/min.Silk through drawing-off, drip washing, centrifugal, obtained 75D/24F spinning cake.Spinning cake compresses and washes through secondary, and cross-linking agent solution compresses and washes, and solidification desulfurization body lotion consists of: soft water: cationic cross linking agent: sodium hydrogensulfite=0.66:0.33:0.01.Retain first to wash together with last, cancel the operation such as desulfurization, pickling, change solidification desulfurization process into, time requirement > 25min, liquid temperature >=75 DEG C.
Compress and wash route
Project Liquid temperature/DEG C Time/min
1 station washing 45 /
2 station solidification desulfurization >75 35
3 station solidification desulfurization >75 35
4 station solidification desulfurization >75 35
5 station washings 45 /
6 station washings Normal temperature /
7 station washings Normal temperature /
8 station washings Normal temperature /
9 station washings Normal temperature /
10 station washings 30 /
11 stations oil 35 /
Compress and wash the fire resistance fibre after having oiled, drying, become cylinder to obtain heat-resistant fireproof viscose filament yarn.
The heat-resistant fireproof viscose filament yarn obtained, its dry fracture strength >=1.85cn/dtex, moisture 8% ~ 15%; still fiber shape can be maintained under 1200 DEG C of aerobic conditions; without melting dropping under hot conditions, silk fabrics can form shielding protection layer, limited oxygen index LOI >=28%.

Claims (1)

1. a preparation method for environment-friendly type thermostable durable flame-retardant fiber, the raw material of described fire resistance fibre is made up of cellulose, fire retardant, cationic cross linking agent, and the ratio of weight and number of each raw material described is:
Cellulose 65 ~ 84
Fire retardant 16 ~ 35
Cationic cross linking agent 1 ~ 3;
The ionic species of described cationic cross linking agent is Ti 4+, RN 3+, Al 3+, Ca 2+the mixture of one or more;
Described fire retardant is silica nitrogen heterocyclic compounds;
The described cellulosic degree of polymerization is 600 ~ 800;
Said method comprising the steps of:
1) preparation of viscose glue stoste is by traditional viscose glue stoste preparation method, by cellulose through soda-dip, squeezing, pulverizing, experienced, sulfonation, filter together, two roads filter, three roads filter, bubble removal step, are prepared into spinning veiscose stoste, i.e. IIIF glue;
2) preparation of Retardant Injection liquid is according to dispersant: 10% alkali lye: fire retardant=(0.05 ~ 0.0769): (0.2 ~ 0.23): the volume ratio of (0.59 ~ 0.69) is allocated, and the Retardant Injection liquid prepared remains in stirring;
3) fire retardant spin before injection by step 1), step 2) the IIIF glue for preparing and the mixing of Retardant Injection liquid, described IIIF glue and Retardant Injection liquid volume ratio are:
IIIF glue 69 ~ 79
Retardant Injection liquid 31 ~ 21;
By dynamic and static state blender before described Retardant Injection liquid injection spinning head, after mixing, obtain anti-flaming viscose;
4) anti-flaming viscose obtained in step 3) is sprayed by spinning head and obtains spinning by spinning, and described spinning obtains fire resistance fibre head product through acid bath, and wherein, shower nozzle aperture is 0.045 ~ 0.065mm, shower nozzle drawing-off 50 ~ 60%, plasticizing drawing-off 50 ~ 100%;
5) concise described fire resistance fibre head product is respectively through washing together, two road washings, and solidification desulfurization, three roads are washed, oiled, and namely obtain described environment-friendly type thermostable durable flame-retardant fiber;
Consisting of of IIIF glue in described step 1:
First fibre 8.1 ~ 9.8%
NaOH 5.4 ~ 7.8%;
The viscosity of described IIIF glue 40 ~ 60 seconds, in the degree of ripeness 14 ~ 16ml of 10% ammonium chloride;
Described dispersant in described step 2 is polyvinyl alcohol, and described alkali lye is sodium hydroxide solution;
In described step 3, the addition manner of fire retardant is for spinning front injection, and before adopting injector or compressed air that Retardant Injection liquid is injected spinning head, dynamic and static state blender mixes glue, consisting of of described anti-flaming viscose:
First fibre 9 ~ 9.5%
Alkali 7.8 ~ 8.1%;
The viscosity >27s of described anti-flaming viscose, with 15%NH 4degree of ripeness 8 ~ the 9ml of Cl meter;
Raw material in acid bath solution in described step 4 comprises sulfuric acid, sodium sulphate, zinc sulfate, and the ratio of weight and number of each raw material described is:
Sulfuric acid 70 ~ 145
Sodium sulphate 220 ~ 350
Zinc sulfate 14 ~ 90;
Described acid bath temperature is 36 DEG C ~ 55 DEG C;
Solidify described in described step 5 in desulfurization, the raw material of body lotion used comprises soft water, cationic cross linking agent and sodium hydrogensulfite, and the ratio of weight and number of each raw material described is:
Soft water 0.66
Cationic cross linking agent 0.33
Sodium hydrogensulfite 0.01;
The temperature of solidifying desulfurization described in described step 5 is 75 ~ 90 DEG C, and the time is 8 ~ 15 minutes.
CN201410039251.0A 2014-01-27 2014-01-27 A kind of environment-friendly type thermostable durable flame-retardant fiber and preparation method thereof Active CN103789858B (en)

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Patentee before: Liu Chengxiu