CN106702512A - Preparation method of poly[bis(methoxyethoxy)phosphazene] blended modified viscose fiber - Google Patents
Preparation method of poly[bis(methoxyethoxy)phosphazene] blended modified viscose fiber Download PDFInfo
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- CN106702512A CN106702512A CN201611120674.0A CN201611120674A CN106702512A CN 106702512 A CN106702512 A CN 106702512A CN 201611120674 A CN201611120674 A CN 201611120674A CN 106702512 A CN106702512 A CN 106702512A
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- phosphonitrile
- methoxypolyethylene glycol
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G79/00—Macromolecular compounds obtained by reactions forming a linkage containing atoms other than silicon, sulfur, nitrogen, oxygen, and carbon with or without the latter elements in the main chain of the macromolecule
- C08G79/02—Macromolecular compounds obtained by reactions forming a linkage containing atoms other than silicon, sulfur, nitrogen, oxygen, and carbon with or without the latter elements in the main chain of the macromolecule a linkage containing phosphorus
- C08G79/025—Polyphosphazenes
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
- D01F2/06—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from viscose
- D01F2/08—Composition of the spinning solution or the bath
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Artificial Filaments (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention relates to the technical fields of synthetic resin and plastic and particularly relates to a preparation method of a poly[bis(methoxyethoxy)phosphazene] blended modified viscose fiber. The preparation method of the poly[bis(methoxyethoxy)phosphazene] blended modified viscose fiber comprises the following steps: (1), synthesizing poly[bis(methoxyethoxy)phosphazene]; (2) performing a purification process on poly[bis(methoxyethoxy)phosphazene]; and (3) preparing a blended flame-retardant viscose fiber. The poly[bis(methoxyethoxy)phosphazene] blended modified viscose fiber prepared by the preparation method has a favorable flame retardant effect, and the flame-retardant modified viscose fiber has a limited oxygen index of 33%.
Description
Technical field
The present invention relates to synthetic resin and plastics arts, and in particular to a kind of methoxypolyethylene glycol phosphonitrile blending and modifying
The preparation method of viscose rayon.
Background technology
Nitrogen, two kinds of elements of phosphorus have synergy at fire-retardant aspect, can not only improve flame retardant effect, and environment is produced
Pollution it is small.In recent years, the emphasis that phosphorus, nitrogen system synergistic fire retardant are developed into halogen-free flame retardants, and phosphazene flame retardant just belongs to
In this kind of nitrogen phosphorus system synergistic fire retardant.Phosphazene compound is that a class has organic and inorganic characteristic compound concurrently, and its skeleton is by nitrogen
Phosphorus singly-bound and nitrogen phosphorus double bond are alternatively formed, and constitute natural nitrogen phosphorus collaboration system, with good heat endurance, anti-flammability, low
Cigarette, hypotoxicity.
On phosphazene flame retardant, although have the report of many pertinent literatures, but focus primarily upon fire-retardant to cyclic phosphazene
The research and development aspect of agent, the research to linear Synthesis, Characterization of Polyphosphazenes fire retardant is still less.
The content of the invention
The present invention is directed to propose a kind of preparation method of methoxypolyethylene glycol phosphonitrile blending and modifying viscose rayon.
Technical program of the present invention lies in：
The preparation method of methoxypolyethylene glycol phosphonitrile blending and modifying viscose rayon, comprises the following steps：
（1）The synthesis of methoxypolyethylene glycol phosphonitrile
Under nitrogen protection, with tetrahydrofuran as solvent, reacted during EGME and metallic sodium are added into there-necked flask；Question response
After end, by the tetrahydrofuran solution above-mentioned there-necked flask of addition of polydichlorophosphazenes, 30 ~ 45min is stirred at reflux at 68 ~ 70 DEG C
Afterwards, methoxypolyethylene glycol phosphonitrile is obtained, most tetrahydrofuran in vacuum distillation removing system adds heptane so that poly- second
Glycol methyl ether phosphonitrile is precipitated out in system, and dropwise addition hydrochloric acid is neutralized to pH value and is about 7, after stirring after 20min, the portion's of removing precipitation
Thing is dissolved in water；
（2）The purifying technique of methoxypolyethylene glycol phosphonitrile
Above-mentioned solution is dialysed in bag filter, 1 distilled water is changed daily, dialysed 3 days, distill solution decompression after 3 days, obtained
Methoxypolyethylene glycol phosphonitrile after to purification；
（3）The preparation of blending fire retardant viscose rayon
Weigh 500 g through maturation, filtering, deaeration viscose glue stoste, by methoxypolyethylene glycol phosphonitrile add viscose glue stoste in, stir
Mix, be added in spinning-drawing machine accumulator after deaeration, as-spun fibre is obtained by spinning, solidification forming, stretching, winding；Again through alkali
Property desulfurization, pickling, washing, drying, obtain final finished fiber.
Described EGME is 1.2 ~ 1.5 with the mol ratio of metallic sodium：1.0.
Described alkaline desulfurization uses the NaOH of 4 g/L, and temperature is 55 ~ 58 DEG C, and the time is 25 ~ 30 min.
Described pickling uses 1.5 g/L HCl, and temperature is 28 ~ 30 DEG C, and the time is 20 ~ 23min.
The technical effects of the invention are that：
The methoxypolyethylene glycol phosphonitrile blending and modifying viscose rayon that the present invention is made has good flame retardant effect, and its is flame-retardant modified
Viscose rayon limited oxygen index is up to 33%.
Specific embodiment
The preparation method of methoxypolyethylene glycol phosphonitrile blending and modifying viscose rayon, comprises the following steps：
Embodiment 1
（1）The synthesis of methoxypolyethylene glycol phosphonitrile
Under nitrogen protection, with tetrahydrofuran as solvent, reacted during EGME and metallic sodium are added into there-necked flask；Question response
After end, by the tetrahydrofuran solution above-mentioned there-necked flask of addition of polydichlorophosphazenes, 30 ~ 45min is stirred at reflux at 68 ~ 70 DEG C
Afterwards, methoxypolyethylene glycol phosphonitrile is obtained, most tetrahydrofuran in vacuum distillation removing system adds heptane so that poly- second
Glycol methyl ether phosphonitrile is precipitated out in system, and dropwise addition hydrochloric acid is neutralized to pH value and is about 7, after stirring after 20min, the portion's of removing precipitation
Thing is dissolved in water；
（2）The purifying technique of methoxypolyethylene glycol phosphonitrile
Above-mentioned solution is dialysed in bag filter, 1 distilled water is changed daily, dialysed 3 days, distill solution decompression after 3 days, obtained
Methoxypolyethylene glycol phosphonitrile after to purification；
（3）The preparation of blending fire retardant viscose rayon
Weigh 500 g through maturation, filtering, deaeration viscose glue stoste, by methoxypolyethylene glycol phosphonitrile add viscose glue stoste in, stir
Mix, be added in spinning-drawing machine accumulator after deaeration, as-spun fibre is obtained by spinning, solidification forming, stretching, winding；Again through alkali
Property desulfurization, pickling, washing, drying, obtain final finished fiber.
Embodiment 2
（1）The synthesis of methoxypolyethylene glycol phosphonitrile
Under nitrogen protection, with tetrahydrofuran as solvent, reacted during EGME and metallic sodium are added into there-necked flask；Question response
After end, by the tetrahydrofuran solution above-mentioned there-necked flask of addition of polydichlorophosphazenes, 30 ~ 45min is stirred at reflux at 68 ~ 70 DEG C
Afterwards, methoxypolyethylene glycol phosphonitrile is obtained, most tetrahydrofuran in vacuum distillation removing system adds heptane so that poly- second
Glycol methyl ether phosphonitrile is precipitated out in system, and dropwise addition hydrochloric acid is neutralized to pH value and is about 7, after stirring after 20min, the portion's of removing precipitation
Thing is dissolved in water；
（2）The purifying technique of methoxypolyethylene glycol phosphonitrile
Above-mentioned solution is dialysed in bag filter, 1 distilled water is changed daily, dialysed 3 days, distill solution decompression after 3 days, obtained
Methoxypolyethylene glycol phosphonitrile after to purification；
（3）The preparation of blending fire retardant viscose rayon
Weigh 500 g through maturation, filtering, deaeration viscose glue stoste, by methoxypolyethylene glycol phosphonitrile add viscose glue stoste in, stir
Mix, be added in spinning-drawing machine accumulator after deaeration, as-spun fibre is obtained by spinning, solidification forming, stretching, winding；Again through alkali
Property desulfurization, pickling, washing, drying, obtain final finished fiber.
Wherein, described EGME and the mol ratio of metallic sodium are 1.2 ~ 1.5：1.0.Described alkaline desulfurization is used
The NaOH of 4 g/L, temperature is 55 ~ 58 DEG C, and the time is 25 ~ 30 min.Described pickling uses 1.5 g/L HCl, and temperature is
28 ~ 30 DEG C, the time is 20 ~ 23min.
Claims (4)
1. the preparation method of methoxypolyethylene glycol phosphonitrile blending and modifying viscose rayon, it is characterised in that：Comprise the following steps：
（1）The synthesis of methoxypolyethylene glycol phosphonitrile
Under nitrogen protection, with tetrahydrofuran as solvent, reacted during EGME and metallic sodium are added into there-necked flask；Question response
After end, by the tetrahydrofuran solution above-mentioned there-necked flask of addition of polydichlorophosphazenes, 30 ~ 45min is stirred at reflux at 68 ~ 70 DEG C
Afterwards, methoxypolyethylene glycol phosphonitrile is obtained, most tetrahydrofuran in vacuum distillation removing system adds heptane so that poly- second
Glycol methyl ether phosphonitrile is precipitated out in system, and dropwise addition hydrochloric acid is neutralized to pH value and is about 7, after stirring after 20min, the portion's of removing precipitation
Thing is dissolved in water；
（2）The purifying technique of methoxypolyethylene glycol phosphonitrile
Above-mentioned solution is dialysed in bag filter, 1 distilled water is changed daily, dialysed 3 days, distill solution decompression after 3 days, obtained
Methoxypolyethylene glycol phosphonitrile after to purification；
（3）The preparation of blending fire retardant viscose rayon
Weigh 500 g through maturation, filtering, deaeration viscose glue stoste, by methoxypolyethylene glycol phosphonitrile add viscose glue stoste in, stir
Mix, be added in spinning-drawing machine accumulator after deaeration, as-spun fibre is obtained by spinning, solidification forming, stretching, winding；Again through alkali
Property desulfurization, pickling, washing, drying, obtain final finished fiber.
2. the preparation method of methoxypolyethylene glycol phosphonitrile blending and modifying viscose rayon according to claim 1, its feature exists
In：Described EGME is 1.2 ~ 1.5 with the mol ratio of metallic sodium：1.0.
3. the preparation method of methoxypolyethylene glycol phosphonitrile blending and modifying viscose rayon according to claim 1, its feature exists
In：Described alkaline desulfurization uses the NaOH of 4 g/L, and temperature is 55 ~ 58 DEG C, and the time is 25 ~ 30 min.
4. the preparation method of methoxypolyethylene glycol phosphonitrile blending and modifying viscose rayon according to claim 1, its feature exists
In：Described pickling uses 1.5 g/L HCl, and temperature is 28 ~ 30 DEG C, and the time is 20 ~ 23min.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611120674.0A CN106702512A (en) | 2016-12-08 | 2016-12-08 | Preparation method of poly[bis(methoxyethoxy)phosphazene] blended modified viscose fiber |
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| CN201611120674.0A CN106702512A (en) | 2016-12-08 | 2016-12-08 | Preparation method of poly[bis(methoxyethoxy)phosphazene] blended modified viscose fiber |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107287667A (en) * | 2017-06-26 | 2017-10-24 | 苏州威尔德工贸有限公司 | A kind of manufacture method of fire-retardant composite silk fiber |
| CN112111792A (en) * | 2020-09-03 | 2020-12-22 | 赛得利(江苏)纤维有限公司 | Automatic control system for viscose temperature |
-
2016
- 2016-12-08 CN CN201611120674.0A patent/CN106702512A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107287667A (en) * | 2017-06-26 | 2017-10-24 | 苏州威尔德工贸有限公司 | A kind of manufacture method of fire-retardant composite silk fiber |
| CN112111792A (en) * | 2020-09-03 | 2020-12-22 | 赛得利(江苏)纤维有限公司 | Automatic control system for viscose temperature |
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