CN106222770A - A kind of terylene chemical fibre fire retardant preparation method - Google Patents
A kind of terylene chemical fibre fire retardant preparation method Download PDFInfo
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- CN106222770A CN106222770A CN201610541832.3A CN201610541832A CN106222770A CN 106222770 A CN106222770 A CN 106222770A CN 201610541832 A CN201610541832 A CN 201610541832A CN 106222770 A CN106222770 A CN 106222770A
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- fire retardant
- chemical fibre
- terylene chemical
- fibre fire
- catalyst
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- 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
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/07—Addition of substances to the spinning solution or to the melt for making fire- or flame-proof filaments
-
- 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
-
- 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
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Medicinal Chemistry (AREA)
- Organic Chemistry (AREA)
- Polymers & Plastics (AREA)
- Health & Medical Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Artificial Filaments (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Multicomponent Fibers (AREA)
Abstract
The invention discloses a kind of terylene chemical fibre fire retardant preparation method, comprise the following steps: trimerization phosphine oxide and uv stabilizer are added in tetraphenyl bisphosphonates, reacts certain time, be prepared as intermediate；Being rendered to by intermediate in blender, at the uniform velocity stir through certain time, temperature, making the trimerization phosphine oxide in intermediate, tetraphenyl bisphosphonates, the ratio of uv stabilizer is 4.5: 1: 0.05, stops stirring；Add a certain amount of catalyst obtaining in intermediate after heated and stirred, then it is carried out the at the uniform velocity stirring of certain time, temperature；When temperature is adjusted to 160 180 degrees Celsius, add a certain amount of phenol and catalyst, through the reaction of certain time；A certain amount of three cyanurates are added in the solution formed；Control certain reaction temperature and the solution formed is carried out end capping reaction, make terylene chemical fibre fire retardant.The invention has the beneficial effects as follows, simple in construction, practical.
Description
Technical field
The present invention relates to terylene chemical fibre and polyester resin, particularly a kind of terylene chemical fibre fire retardant preparation method.
Background technology
Being used for polyester dacron fiber halogen-containing flame retardant the earliest is a kind of inorganic fire-retarded addition manner, due in combustion process
The a large amount of toxic gas of middle release, the had carcinogenecity even having, the later stage has invented again halogen-free flameproof, in halogen-free flame retardants, contains
Phosphorus fire retardant, owing to producing little toxic gas, is widely used, and traditional little molecule halogen-free flame retardants is used for producing
There have again in the middle of product to be poor with polymer compatibility, it is easy to product melts uneven, and can reduce the mechanical strength of polymer, later stage
The processing process produced in the application with high phosphorus-containing flame-retardant material that polyester material reacts by reactor with esterifying liquid
The complicated processing cost wasting of resources, meanwhile, being used for polyster fibre halogen-containing flame retardant the earliest is a kind of inorganic fire-retarded addition manner,
Owing to discharging a large amount of toxic gas in combustion, the had carcinogenecity even having, the later stage has invented again halogen-free flameproof, in nothing
In halogen fire retardant, phosphonium flame retardant, owing to producing little toxic gas, is widely used, traditional little molecule Halogen
It is poor with polymer compatibility that fire retardant has again in the middle of product, it is easy to product melts uneven, and can reduce polymer
Mechanical strength, being produced in the application with high phosphorus-containing flame-retardant material that polyester material reacts by reactor with esterifying liquid of later stage
The processing process complicated processing cost wasting of resources, spinnability is poor, it is impossible to directly make an addition to regenerative piece of polyester bottle, it is necessary to former
Material spinning fibre.
Summary of the invention
The invention aims to solve the problems referred to above, devise a kind of terylene chemical fibre fire retardant preparation method.
Realize above-mentioned purpose the technical scheme is that, a kind of terylene chemical fibre fire retardant preparation method, this preparation method
Comprise the following steps:
(1) intermediate is prepared: add in tetraphenyl bisphosphonates by trimerization phosphine oxide and uv stabilizer, react certain time,
It is prepared as intermediate；
(2) heated and stirred: rendered to by intermediate in blender, at the uniform velocity stirs through certain time, temperature, makes intermediate
In trimerization phosphine oxide, tetraphenyl bisphosphonates, the ratio of uv stabilizer be 4.5: 1: 0.05, stop stirring；
(3) catalyst is added: add a certain amount of catalyst obtaining in intermediate after heated and stirred, then it is carried out
Certain time, the at the uniform velocity stirring of temperature；
(4) add phenol and catalyst: when temperature is adjusted to 160-180 degree Celsius, add a certain amount of phenol and urge
Agent, through the reaction of certain time；
(5) three cyanurates are added: the solution in step (4) adds a certain amount of three cyanurates；
(6) end capping reaction: control the solution that step (5) forms by certain reaction temperature and carry out end capping reaction, make terylene
Chemical fibre fire retardant.
In step (2), the described response time is about 4 hours.
In step (2), described reaction temperature is 100-120 degree Celsius.
In step (3), the described response time is about 4 hours.
In step (3), the quantity that described catalyst uses is about the 3% of added tetraphenyl bisphosphonates quantity.
In step (4), the described response time is 1-1.5 hour.
In step (4), the ratio that described interpolation phenol forms solution with step (3) is 1: 3.8-4.
In step (4), described interpolation catalyst is that step (3) forms the 1% of solution volume.
In step (5), the ratio that described interpolation three cyanurate forms solution with step (4) is 1: 0.8-1.2.
In step (6), described reaction temperature is 200-240 degree Celsius.
Utilizing the terylene chemical fibre fire retardant preparation method that technical scheme makes, this terylene chemical fibre fire retardant is a kind of
Through the halogen-free environmental response type permanent fire retardant high molecular weight flame retardant of special warfare processing, it is that the macromolecule of a kind of function admirable has
Machine phosphorous-nitrogen system bittern-free environmental protection fire retarding agent, has higher stability, non-oxidizability and excellent resistance to water, is that a kind of high reaction is total to
Poly-type fire retardant, owing to this fire retardant has phosphorus nitrogen molecular to be good for fire resistance than general organic phosphate flame-retardant effect more preferably, avirulence,
Non-stimulated to skin, fire resistance arbitrarily can be added according to fire-retardant coefficient, can be directly added into polyester slice, and regenerative piece of polyester bottle is straight
Connect spinning (break through reclaiming bottle piece and cannot spin fire resistance fibre), it is not necessary to react through reactor, screw rod can be directly over and directly add,
Good spinnability, increases spinning elastic, meanwhile, has good heat and UV stability. and only need a dose point just can reach UL-
94, V-2, or the standard .UV stability of V-0 even can strengthen the adhesion with polyester.Forming temperature be fusing, immediately and
Polyester combines, and will not destroy polyester primary characteristic and cause reducing outflow.There is the strongest heat stability and polyester will not be destroyed
Quality, make simultaneously normal complexion molding be easier to.It addition, it can also reduce mould residual.Forming temperature scope can be according to heat
The use of stabilizer (epoxy, or organic tin stabilizer, brucite, fragrant kind antioxidant, chelating agen etc.) and strengthen, greatly reduce
Produce fire resistance fibre processing cost, the processing charges lowering 500-700 unit to I haven't seen you for ages per ton, add economic benefit.
Accompanying drawing explanation
Fig. 1 is the structural representation of terylene chemical fibre fire retardant preparation method of the present invention；
Detailed description of the invention
Below in conjunction with the accompanying drawings the present invention is specifically described, as it is shown in figure 1, a kind of terylene chemical fibre fire retardant preparation side
Method, this preparation method comprises the following steps: add in tetraphenyl bisphosphonates by trimerization phosphine oxide and uv stabilizer, reaction one timing
Between, it is prepared as intermediate；Intermediate is rendered in blender, at the uniform velocity stir through certain time, temperature, make in intermediate
Trimerization phosphine oxide, tetraphenyl bisphosphonates, the ratio of uv stabilizer are 4.5: 1: 0.05, stop stirring；After heated and stirred
Obtain in intermediate and add a certain amount of catalyst, then it is carried out the at the uniform velocity stirring of certain time, temperature；Temperature is adjusted to
When 160-180 degree Celsius, add a certain amount of phenol and catalyst, through the reaction of certain time；Solution in step (4)
A certain amount of three cyanurates of middle interpolation；Control the solution that step (5) forms by certain reaction temperature and carry out end capping reaction, make
Terylene chemical fibre fire retardant；In step (2), the described response time is about 4 hours；In step (2), described reaction temperature is 100-
120 degrees Celsius；In step (3), the described response time is about 4 hours；In step (3), the quantity that described catalyst uses is
About the 3% of added tetraphenyl bisphosphonates quantity；In step (4), the described response time is 1-1.5 hour；Step (4)
In, the ratio that described interpolation phenol forms solution with step (3) is 1: 3.8-4；In step (4), described interpolation catalyst is step
Suddenly (3) form the 1% of solution volume；In step (5), the ratio that described interpolation three cyanurate forms solution with step (4) is 1
∶0.8-1.2；In step (6), described reaction temperature is 200-240 degree Celsius.
The feature of the present embodiment is, comprises the following steps: trimerization phosphine oxide and uv stabilizer are added tetraphenyl di 2 ethylhexyl phosphonic acid
In ester, react certain time, be prepared as intermediate；Intermediate is rendered in blender, at the uniform velocity stir through certain time, temperature
Mixing, making the trimerization phosphine oxide in intermediate, tetraphenyl bisphosphonates, the ratio of uv stabilizer is 4.5: 1: 0.05, stops stirring；?
Obtain in intermediate after heated and stirred and add a certain amount of catalyst, then it is carried out the at the uniform velocity stirring of certain time, temperature；
When temperature is adjusted to 160-180 degree Celsius, add a certain amount of phenol and catalyst, through the reaction of certain time；In step
Suddenly the solution in (4) adds a certain amount of three cyanurates；Control the solution that step (5) forms by certain reaction temperature to carry out
End capping reaction, makes terylene chemical fibre fire retardant, and a kind of halogen-free environmental through special warfare processing of this terylene chemical fibre fire retardant is anti-
Answer type permanent fire retardant high molecular weight flame retardant, be the macromolecule organophosphor nitrogen system bittern-free environmental protection fire retarding agent of a kind of function admirable, have
Higher stability, non-oxidizability and excellent resistance to water, be a kind of high reaction copoly type fire retardant, owing to this fire retardant has phosphorus
It is more preferable than general organic phosphate flame-retardant effect that nitrogen molecular is good for fire resistance, and avirulence, non-stimulated to skin, fire resistance can basis
Fire-retardant coefficient arbitrarily adds, and can be directly added into polyester slice, and regenerative piece of polyester bottle direct fabrics (are broken through reclaiming bottle piece and cannot be spun resistance
Combustion fiber), it is not necessary to react through reactor, screw rod can be directly over and directly add, good spinnability, increase spinning elastic, meanwhile,
There is good heat and UV stability. only need a dose point just can reach the standard .UV stability of UL-94, V-2, or V-0 very
To strengthening the adhesion with polyester.It is fusing at forming temperature, combines with polyester immediately, polyester primary characteristic will not be destroyed
Flow out with causing reducing.There is the strongest heat stability and the quality of polyester will not be destroyed, making normal complexion molding be easier to simultaneously.
It addition, it can also reduce mould residual.Forming temperature scope can be according to heat stabilizer (epoxy, or organic tin stabilizer, water
Talcum, fragrant kind antioxidant, chelating agen etc.) use and strengthen, greatly reduce production fire resistance fibre processing cost, per ton to I haven't seen you for ages
Lower the processing charges of 500-700 unit, add economic benefit.
In the present embodiment, trimerization phosphine oxide is added tetraphenyl diphosphine within a period of time by the preparation method of this fire retardant
Acid esters, and uv stabilizer makes intermediate, the scope of reaction temperature 100-120 degree, uniform through high-speed stirred, the response time 4 is little
Time about, trimerization phosphine oxide and four basic bisphosphates, uv stabilizer proportioning, about 4.5: 1: 0.05, stops stirring, is passing through
Obtaining after heated and stirred in intermediate and add catalyst, the quantity used is about the 3% of added tetraphenyl bisphosphonates, warp
After crossing reaction in 4 hours, control temperature to add phenol, additional proportion 1: 3.8-4 at 160-180 degree, add catalyst and be about 1%
Left and right, in 1-1.5 hour response time, the 3rd step adds three cyanurates, adding proportion be early stage addition 1: 0.8-1.2 it
Between, carrying out end capping reaction, reaction temperature is between 200-240 degree, and this product has good heat and UV stability. only need a bit
Dosage just can reach the standard of UL-94, V-2, or V-0.
In the present embodiment, directly can be directly used in monofilament polyester through Screw Extrusion by batch mixing to produce, the most
In monofilament produces, it is possible to directly make flame retardant polyester section with regenerative piece of polyester bottle through batch mixing.
In the present embodiment, UV stability even can strengthen the adhesion with polyester, melts when forming temperature, with
I.e. combine with polyester, polyester primary characteristic will not be destroyed and cause reducing outflow, there is the strongest heat stability and will not destroy
The quality of polyester, makes normal complexion molding be easier to simultaneously, it addition, it can also reduce mould residual, forming temperature scope can root
Strengthen according to the use of heat stabilizer.
In the present embodiment, a kind of halogen-free environmental response type through special warfare processing of this terylene chemical fibre fire retardant is forever
Flame-retardant high-molecular fire retardant, is the macromolecule organophosphor nitrogen system bittern-free environmental protection fire retarding agent of a kind of function admirable, has higher for a long time
Stability, non-oxidizability and excellent resistance to water, be a kind of high reaction copoly type fire retardant, and avirulence, stingless to skin
Swashing, fire resistance arbitrarily can be added according to fire-retardant coefficient, can be directly added into polyester slice, regenerative piece of polyester bottle direct fabrics, nothing
Need to react through reactor, screw rod can be directly over and directly add, good spinnability, increase spinning elastic.
Technique scheme only embodies the optimal technical scheme of technical solution of the present invention, those skilled in the art
Some variations may made some of which part all embody the principle of the present invention, belong to protection scope of the present invention it
In.
Claims (10)
1. a terylene chemical fibre fire retardant preparation method, it is characterised in that this preparation method comprises the following steps:
(1) intermediate is prepared: add in tetraphenyl bisphosphonates by trimerization phosphine oxide and uv stabilizer, react certain time, preparation
Become intermediate；
(2) heated and stirred: rendered to by intermediate in blender, at the uniform velocity stirs through certain time, temperature, makes in intermediate
Trimerization phosphine oxide, tetraphenyl bisphosphonates, the ratio of uv stabilizer are 4.5: 1: 0.05, stop stirring；
(3) catalyst is added: add a certain amount of catalyst obtaining in intermediate after heated and stirred, then it is carried out necessarily
Time, the at the uniform velocity stirring of temperature；
(4) phenol and catalyst are added: when temperature is adjusted to 160-180 degree Celsius, add a certain amount of phenol and catalyst,
Reaction through certain time；
(5) three cyanurates are added: the solution in step (4) adds a certain amount of three cyanurates；
(6) end capping reaction: control the solution that step (5) forms by certain reaction temperature and carry out end capping reaction, make terylene chemical fibre
Fire retardant.
A kind of terylene chemical fibre fire retardant preparation method the most according to claim 1, it is characterised in that in step (2), described
Response time is about 4 hours.
A kind of terylene chemical fibre fire retardant preparation method the most according to claim 1, it is characterised in that in step (2), described
Reaction temperature is 100-120 degree Celsius.
4. according to a kind of terylene chemical fibre fire retardant preparation method described described in claim, it is characterised in that in step (3),
The described response time is about 4 hours.
A kind of terylene chemical fibre fire retardant preparation method the most according to claim 1, it is characterised in that in step (3), described
The quantity that catalyst uses is about the 3% of added tetraphenyl bisphosphonates quantity.
A kind of terylene chemical fibre fire retardant preparation method the most according to claim 1, it is characterised in that in step (4), described
Response time is 1-1.5 hour.
A kind of terylene chemical fibre fire retardant preparation method the most according to claim 1, it is characterised in that in step (4), described
The ratio adding phenol and step (3) formation solution is 1: 3.8-4.
A kind of terylene chemical fibre fire retardant preparation method the most according to claim 1, it is characterised in that in step (4), described
Interpolation catalyst is that step (3) forms the 1% of solution volume.
A kind of terylene chemical fibre fire retardant preparation method the most according to claim 1, it is characterised in that in step (5), described
The ratio adding three cyanurates and step (4) formation solution is 1: 0.8-1.2.
A kind of terylene chemical fibre fire retardant preparation method the most according to claim 1, it is characterised in that in step (6), institute
State reaction temperature and be 200-240 degree Celsius.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610541832.3A CN106222770A (en) | 2016-07-05 | 2016-07-05 | A kind of terylene chemical fibre fire retardant preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610541832.3A CN106222770A (en) | 2016-07-05 | 2016-07-05 | A kind of terylene chemical fibre fire retardant preparation method |
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| CN106222770A true CN106222770A (en) | 2016-12-14 |
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| CN201610541832.3A Pending CN106222770A (en) | 2016-07-05 | 2016-07-05 | A kind of terylene chemical fibre fire retardant preparation method |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1888015A (en) * | 2006-06-05 | 2007-01-03 | 南京师范大学 | Prepn of fire retardant resorcinol tetraphenyldiphosphate |
-
2016
- 2016-07-05 CN CN201610541832.3A patent/CN106222770A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1888015A (en) * | 2006-06-05 | 2007-01-03 | 南京师范大学 | Prepn of fire retardant resorcinol tetraphenyldiphosphate |
Non-Patent Citations (2)
| Title |
|---|
| 蒋明访等: ""阻燃剂三（二苯基磷酸）异氰酸酯的合成及其在聚氨酯中的应用"", 《塑料工业》 * |
| 高存生等: ""氯化磷酸二苯酯的合成和结构表征"", 《化学研究》 * |
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Application publication date: 20161214 |