CN107501559A - A kind of phosphorus flame retardant applied in plastic products - Google Patents

A kind of phosphorus flame retardant applied in plastic products Download PDF

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Publication number
CN107501559A
CN107501559A CN201710807158.3A CN201710807158A CN107501559A CN 107501559 A CN107501559 A CN 107501559A CN 201710807158 A CN201710807158 A CN 201710807158A CN 107501559 A CN107501559 A CN 107501559A
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China
Prior art keywords
parts
plastic products
flame retardant
phosphorus flame
ome
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CN201710807158.3A
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Chinese (zh)
Inventor
程聚光
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Xuancheng City Trooyawn Refined Chemical Industry Co Ltd
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Xuancheng City Trooyawn Refined Chemical Industry Co Ltd
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Priority to CN201710807158.3A priority Critical patent/CN107501559A/en
Publication of CN107501559A publication Critical patent/CN107501559A/en
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/04Polysiloxanes
    • C08G77/14Polysiloxanes containing silicon bound to oxygen-containing groups
    • C08G77/18Polysiloxanes containing silicon bound to oxygen-containing groups to alkoxy or aryloxy groups
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/04Polysiloxanes
    • C08G77/38Polysiloxanes modified by chemical after-treatment
    • C08G77/382Polysiloxanes modified by chemical after-treatment containing atoms other than carbon, hydrogen, oxygen or silicon
    • C08G77/395Polysiloxanes modified by chemical after-treatment containing atoms other than carbon, hydrogen, oxygen or silicon containing phosphorus

Abstract

The present invention relates to the research and development technology field of fire retardant, discloses a kind of phosphorus flame retardant applied in plastic products, is made up in parts by weight of following component:80 90 parts of diethyl phosphite, 70 75 parts of epoxy silicone, 18 22 parts of ethylenediamine tetra-acetic acid, 10 15 parts of triethylamine, 46 parts of HMDO, 10 15 parts of distilled water, the addition of containing silicone resin improves the fire resistance of system in compound flame retardant, the Si O Si network structures formed after decomposition add the heat endurance of surface layer of charcoal, the phosphorus flame retardant that the present invention is prepared is applied on plastic products, addition is extremely low, burning grade can reach 0 grade of FV, every fire resistance index of plastic products can not only be improved, the mechanical property of plastics can also be improved, including elongation at break, shock resistance.

Description

A kind of phosphorus flame retardant applied in plastic products
Technical field
The invention belongs to the research and development technology field of fire retardant, and in particular to a kind of phosphorous flame-retardant applied in plastic products Agent.
Background technology
With the development of modernization science and technology, high polymer material is applied to every field more and more widely.But this A little materials are typically all inflammable or flammable, thus cause fire incident, it has also become the social concern of people's general concern.Due to Growing to even greater heights for fire-retardant fireproof cry and being gradually improved for flame retardant regulation, have directly facilitated fire retarding chimical in world wide Research, development and production application.In order to solve the resistance to combustion of synthetic material, suppression cigarette, it is less toxic the problems such as, it is ensured that what synthetic material used Security, most efficient method are a kind of efficient, nontoxic fire retardants of addition.Fire retardant, assign combustible polymers flame retardancy Functional aid, primarily directed to the Principle And Method of Flame Retardation Design of high polymer material, fire retardant has polytype, be divided into by application method and adding Add type fire retardant and reactive flame retardant.
Caloric value is big when plastic products meet fire burning, and burning velocity is fast, produces largely molten entropy, and with smoke phenomenon, pole Easy propagating flame, easily occurs fire, brings the infringement of life and property, with the improvement of people ' s living standards and ring The enhancing of consciousness, the requirement more and more higher for plastic flame performance are protected, common fire retardant can not meet wanting for people Ask.
The content of the invention
The purpose of the present invention is to be directed to the problem of existing, there is provided a kind of phosphorus flame retardant applied in plastic products, Every fire resistance index of plastic products can not only be improved, additionally it is possible to improve the mechanical property of plastics, including extension at break Rate, shock resistance.
The present invention is achieved by the following technical solutions:
A kind of phosphorus flame retardant applied in plastic products, is made up of following component in parts by weight:Diethyl phosphite 80-90 parts, epoxy silicone 70-75 parts, ethylenediamine tetra-acetic acid 18-22 parts, triethylamine 10-15 parts, HMDO 4- 6 parts, distilled water 10-15 parts, it reduces the preparation method of reaction and comprised the following steps:
(1)0.6 mole of diethyl phosphite is encased in 1000 milliliters of three-necked flask, uses heating water bath to 60-70 DEG C, 0.2 mole of freshly prepd epoxy silicone, 150-180 millis is added dropwise under 360-400 revs/min of mechanical agitation slurry stirring The ethylenediamine tetra-acetic acid and the triethylamine of 100-120 milliliters risen, is reacted under nitrogen protection;
(2)When reaction progress to system color changes, regulation solution pH value is 6.8-7.0, adds water and the silicon of hexamethyl two Oxygen alkane binds, and continues stirring reaction 1-2 hours, is evaporated under reduced pressure and removes solvent, and it is each using water and tetrahydrofuran respectively to take out solid Washing 3-4 times, vacuum drying obtain product as light yellow solid.
Further described as to such scheme, the preparation method of the freshly prepd epoxy silicone is:
(1)It is 20-30% sodium hydroxide water that mass concentration is added into the three-necked flask with reflux condensing tube and mechanical agitation oar Solution, addition accounts for the 30-35% of flask volume, after being heated to 45-50 DEG C, adds the toluene for accounting for flask volume 10-15%;
(2)After stirring reaction 10-15 minutes, PhSi (OMe) is added dropwise using constant pressure funnel3And Ph2Si(OMe)2, drop After adding, continue to be heated to reflux 2-3 hours, after reaction terminates, being washed to neutrality using saturated common salt, using Rotary Evaporators Organic phase is distillated, surplus materials is the epoxy silicone.
Further described as to such scheme, step(2)Described in during ethylenediamine tetra-acetic acid, triethylamine, drop Acceleration Control is in 8-10 drops/sec of scope, and reaction temperature is in 70-80 DEG C of scope.
Further described as to such scheme, the PhSi (OMe)3And Ph2Si(OMe)2Mixed proportion be 1.5-1.7:1, addition is the 8-10% of flask volume.
Further described as to such scheme, addition mass fraction of the fire retardant in plastic products is 0.10-0.15%。
The present invention has advantages below compared with prior art:Exist to solve existing fire-retardant for plastic during fire-retardant Insufficient problem, the invention provides a kind of phosphorus flame retardant applied in plastic products, containing silicone resin in compound flame retardant Addition improve the fire resistance of system, the Si-O-Si network structures formed after decomposition add the thermostabilization of surface layer of charcoal Property, the phosphorus flame retardant that is prepared of the present invention applied on plastic products, and addition is extremely low, and burning grade can reach FV-0 Level, every fire resistance index of plastic products can not only be improved, additionally it is possible to improve the mechanical property of plastics, including fracture is stretched Long rate, shock resistance.
Embodiment
With reference to specific embodiment, the invention will be further described.
Embodiment 1
A kind of phosphorus flame retardant applied in plastic products, is made up of following component in parts by weight:Diethyl phosphite 80 parts, 70 parts of epoxy silicone, 18 parts of ethylenediamine tetra-acetic acid, 10 parts of triethylamine, 4 parts of HMDO, distilled water 10 Part, it reduces the preparation method of reaction and comprised the following steps:
(1)0.6 mole of diethyl phosphite is encased in 1000 milliliters of three-necked flask, using heating water bath to 60 DEG C, 0.2 mole of freshly prepd epoxy silicone, 150 milliliters of ethylenediamine tetraacetic is added dropwise under 360 revs/min of mechanical agitation slurry stirring Acetic acid and 100 milliliters of triethylamine, are reacted under nitrogen protection;
(2)When reaction progress to system color changes, regulation solution pH value is 6.8, add water and HMDO Bind, continue stirring reaction 1 hour, be evaporated under reduced pressure and remove solvent, take out solid respectively using the respectively washing 3 of water and tetrahydrofuran Secondary, vacuum drying obtains product as light yellow solid.
Further described as to such scheme, the preparation method of the freshly prepd epoxy silicone is:
(1)It is that 20% sodium hydroxide is water-soluble that mass concentration is added into the three-necked flask with reflux condensing tube and mechanical agitation oar Liquid, addition account for the 30% of flask volume, after being heated to 45 DEG C, add the toluene for accounting for flask volume 10%;
(2)After stirring reaction 10 minutes, PhSi (OMe) is added dropwise using constant pressure funnel3And Ph2Si(OMe)2, it is added dropwise After, continue to be heated to reflux 2 hours, after reaction terminates, be washed to neutrality using saturated common salt, will be had using Rotary Evaporators Machine mutually distillates, and surplus materials is the epoxy silicone.
Further described as to such scheme, step(2)Described in during ethylenediamine tetra-acetic acid, triethylamine, drop Acceleration Control is in 8-10 drops/sec of scope, and reaction temperature is in 70-80 DEG C of scope.
Further described as to such scheme, the PhSi (OMe)3And Ph2Si(OMe)2Mixed proportion be 1.5:1, addition is the 8% of flask volume.
Further described as to such scheme, addition mass fraction of the fire retardant in plastic products is 0.10%。
Embodiment 2
A kind of phosphorus flame retardant applied in plastic products, is made up of following component in parts by weight:Diethyl phosphite 85 parts, 73 parts of epoxy silicone, 20 parts of ethylenediamine tetra-acetic acid, 12 parts of triethylamine, 5 parts of HMDO, distilled water 12 Part, it reduces the preparation method of reaction and comprised the following steps:
(1)0.6 mole of diethyl phosphite is encased in 1000 milliliters of three-necked flask, using heating water bath to 65 DEG C, 0.2 mole of freshly prepd epoxy silicone, 160 milliliters of ethylenediamine tetraacetic is added dropwise under 380 revs/min of mechanical agitation slurry stirring Acetic acid and 110 milliliters of triethylamine, are reacted under nitrogen protection;
(2)When reaction progress to system color changes, regulation solution pH value is 6.9, adds water and HMDO Bind, continue stirring reaction 1.5 hours, be evaporated under reduced pressure and remove solvent, take out solid respectively using the respectively washing 3 of water and tetrahydrofuran Secondary, vacuum drying obtains product as light yellow solid.
Further described as to such scheme, the preparation method of the freshly prepd epoxy silicone is:
(1)It is that 25% sodium hydroxide is water-soluble that mass concentration is added into the three-necked flask with reflux condensing tube and mechanical agitation oar Liquid, addition account for the 32% of flask volume, after being heated to 48 DEG C, add the toluene for accounting for flask volume 12%;
(2)After stirring reaction 12 minutes, PhSi (OMe) is added dropwise using constant pressure funnel3And Ph2Si(OMe)2, it is added dropwise After, continue to be heated to reflux 2.5 hours, after reaction terminates, neutrality is washed to using saturated common salt, will using Rotary Evaporators Organic phase distillates, and surplus materials is the epoxy silicone.
Further described as to such scheme, step(2)Described in during ethylenediamine tetra-acetic acid, triethylamine, drop Acceleration Control is in 8-10 drops/sec of scope, and reaction temperature is in 70-80 DEG C of scope.
Further described as to such scheme, the PhSi (OMe)3And Ph2Si(OMe)2Mixed proportion be 1.6:1, addition is the 9% of flask volume.
Further described as to such scheme, addition mass fraction of the fire retardant in plastic products is 0.12%。
Embodiment 3
A kind of phosphorus flame retardant applied in plastic products, is made up of following component in parts by weight:Diethyl phosphite 90 parts, 75 parts of epoxy silicone, 22 parts of ethylenediamine tetra-acetic acid, 15 parts of triethylamine, 6 parts of HMDO, 15 parts of distilled water, It reduces the preparation method of reaction and comprised the following steps:
(1)0.6 mole of diethyl phosphite is encased in 1000 milliliters of three-necked flask, using heating water bath to 70 DEG C, 0.2 mole of freshly prepd epoxy silicone, 180 milliliters of ethylenediamine tetraacetic is added dropwise under 400 revs/min of mechanical agitation slurry stirring Acetic acid and 120 milliliters of triethylamine, are reacted under nitrogen protection;
(2)When reaction progress to system color changes, regulation solution pH value is 7.0, adds water and HMDO Bind, continue stirring reaction 2 hours, be evaporated under reduced pressure and remove solvent, take out solid respectively using the respectively washing 4 of water and tetrahydrofuran Secondary, vacuum drying obtains product as light yellow solid.
Further described as to such scheme, the preparation method of the freshly prepd epoxy silicone is:
(1)It is that 30% sodium hydroxide is water-soluble that mass concentration is added into the three-necked flask with reflux condensing tube and mechanical agitation oar Liquid, addition account for the 35% of flask volume, after being heated to 50 DEG C, add the toluene for accounting for flask volume 15%;
(2)After stirring reaction 15 minutes, PhSi (OMe) is added dropwise using constant pressure funnel3And Ph2Si(OMe)2, it is added dropwise After, continue to be heated to reflux 3 hours, after reaction terminates, be washed to neutrality using saturated common salt, will be had using Rotary Evaporators Machine mutually distillates, and surplus materials is the epoxy silicone.
Further described as to such scheme, step(2)Described in during ethylenediamine tetra-acetic acid, triethylamine, drop Acceleration Control is in 8-10 drops/sec of scope, and reaction temperature is in 70-80 DEG C of scope.
Further described as to such scheme, the PhSi (OMe)3And Ph2Si(OMe)2Mixed proportion be 1.7:1, addition is the 10% of flask volume.
Further described as to such scheme, addition mass fraction of the fire retardant in plastic products is 0.15%。
Comparative example 1
With differing only in for embodiment 1, the parts by weight of diethyl phosphite and epoxy silicone are respectively:80 parts, 60 parts, its It is remaining to be consistent.
Comparative example 2
With differing only in for embodiment 2, the parts by weight of diethyl phosphite and epoxy silicone are respectively:85 parts, 80 parts, its It is remaining to be consistent.
Comparative example 3
With differing only in for embodiment 3, the parts by weight of diethyl phosphite and epoxy silicone are respectively:90 parts, 100 parts, Remaining is consistent.
Contrast experiment
Fire retardant is prepared using embodiment 1-3 method processing respectively, while using existing Silicone-containing Flame Retardant as control, application Fire retardant prepared by each group, is added in same plastic products, and addition mass percent is 0.15%, by making for each group fire retardant It is compared with effect, effect is as shown in the table:
Project Tensile strength(MPa) Impact strength(KJ/m2 Limited oxygen index(%) Fire-fighting efficiency improves(%)
Embodiment 1 35.4 8.2 42.3 20
Embodiment 2 35.9 8.5 42.8 25
Embodiment 3 35.6 8.3 42.6 23
Comparative example 1 30.5 7.2 30.5 11
Comparative example 2 31.0 7.6 30.9 13
Comparative example 3 30.2 7.0 29.1 7
Control group 29.8 6.9 28.3 Control
By relatively:The phosphorus flame retardant that the present invention is prepared is applied on plastic products, and addition is extremely low, burning etc. Level can reach FV-0 levels, can not only improve every fire resistance index of plastic products, additionally it is possible to improve the mechanics of plastics Performance, including elongation at break, shock resistance.

Claims (5)

1. a kind of phosphorus flame retardant applied in plastic products, it is characterised in that be made up in parts by weight of following component: Diethyl phosphite 80-90 parts, epoxy silicone 70-75 parts, ethylenediamine tetra-acetic acid 18-22 parts, triethylamine 10-15 parts, pregnancy Base disiloxane 4-6 parts, distilled water 10-15 parts, it reduces the preparation method of reaction and comprised the following steps:
(1)0.6 mole of diethyl phosphite is encased in 1000 milliliters of three-necked flask, uses heating water bath to 60-70 DEG C, 0.2 mole of freshly prepd epoxy silicone, 150-180 millis is added dropwise under 360-400 revs/min of mechanical agitation slurry stirring The ethylenediamine tetra-acetic acid and the triethylamine of 100-120 milliliters risen, is reacted under nitrogen protection;
(2)When reaction progress to system color changes, regulation solution pH value is 6.8-7.0, adds water and the silicon of hexamethyl two Oxygen alkane binds, and continues stirring reaction 1-2 hours, is evaporated under reduced pressure and removes solvent, and it is each using water and tetrahydrofuran respectively to take out solid Washing 3-4 times, vacuum drying obtain product as light yellow solid.
2. a kind of phosphorus flame retardant applied in plastic products as claimed in claim 1, it is characterised in that described freshly prepd The preparation method of epoxy silicone is:
(1)It is 20-30% sodium hydroxide water that mass concentration is added into the three-necked flask with reflux condensing tube and mechanical agitation oar Solution, addition accounts for the 30-35% of flask volume, after being heated to 45-50 DEG C, adds the toluene for accounting for flask volume 10-15%;
(2)After stirring reaction 10-15 minutes, PhSi (OMe) is added dropwise using constant pressure funnel3And Ph2Si(OMe)2, drop After adding, continue to be heated to reflux 2-3 hours, after reaction terminates, being washed to neutrality using saturated common salt, using Rotary Evaporators Organic phase is distillated, surplus materials is the epoxy silicone.
A kind of 3. phosphorus flame retardant applied in plastic products as claimed in claim 1, it is characterised in that step(2)Middle institute During stating ethylenediamine tetra-acetic acid, triethylamine, rate of addition is controlled in 8-10 drops/sec of scope, and reaction temperature is in 70-80 DEG C of model Enclose.
A kind of 4. phosphorus flame retardant applied in plastic products as claimed in claim 2, it is characterised in that the PhSi (OMe)3And Ph2Si(OMe)2Mixed proportion be 1.5-1.7:1, addition is the 8-10% of flask volume.
5. a kind of phosphorus flame retardant applied in plastic products as claimed in claim 1, it is characterised in that the fire retardant exists Addition mass fraction in plastic products is 0.10-0.15%.
CN201710807158.3A 2017-09-08 2017-09-08 A kind of phosphorus flame retardant applied in plastic products Pending CN107501559A (en)

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