CN107365433B - Hyperbranched phosphorous modification infusorial earth fire retardant of one kind and preparation method thereof - Google Patents
Hyperbranched phosphorous modification infusorial earth fire retardant of one kind and preparation method thereof Download PDFInfo
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- CN107365433B CN107365433B CN201710574089.6A CN201710574089A CN107365433B CN 107365433 B CN107365433 B CN 107365433B CN 201710574089 A CN201710574089 A CN 201710574089A CN 107365433 B CN107365433 B CN 107365433B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L7/00—Compositions of natural rubber
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
Abstract
The present invention relates to a kind of hyperbranched phosphorous modification infusorial earth fire retardants and preparation method thereof, are prepared using the raw material of following parts by weight of component：Natural rubber matrix：100, vulcanizing agent：2~3, accelerating agent：1~1.5, stearic acid：0.5~1.0, zinc oxide：3~5, anti-aging agent：1~3, hyperbranched modification infusorial earth：10~15, said components are put in proportion into open mill, is kneaded under conditions of temperature is 30~50 DEG C, that is, obtains hyperbranched phosphorous modification infusorial earth fire retardant.Compared with prior art, the present invention, which has, reduces solution viscosity, the dispersion performance of fire retardant is improved, the advantages that making it easier to be added in material.
Description
Technical field
The present invention relates to a kind of preparation methods of fire retardant, fire-retardant more particularly, to a kind of hyperbranched phosphorous modification infusorial earth
Agent and preparation method thereof.
Background technology
Fire threatens always the safety of life and property of people, and the etesian fire in China is about 130,000, puts down
It loses close to 20,000,000,000 yuan, the loss in the injury and property of body is brought to the people.In order to solve this problem,
Using can prevent or the material of retarded combustion has become a kind of trend, people were in some traffic-intensives in recent years
Fire proofing has been used in public place and important building.For fire proofing compares traditional material, need to only it pay more a small amount of
Cost it is prevented that huge property loss.It prepares fire proofing and is broadly divided into that the fire-retardant, additive of grafting is fire-retardant and coating resistance
Combustion.
Fire retardant is a kind of substance for the flame retardant property for being added in high polymer, capable of significantly improving material.Fire retardant
Since it is with lower cost and convenient addition application method, it is widely used in fire proofing.Fire retardant and resistance
The fire retardant mechanism that combustion high molecular material is combined by gas phase, solid phase or both is fire-retardant to achieve the purpose that, to a certain degree
On can make high polymer burning caused by harm be reduced to minimum, to reduce fire caused by life and property loss.Therefore it grinds
Cheap, efficient fire retardant is made, the flame retardant effect of material is improved, improves the fire-protection rating of building, for urban safety and warp
Ji develops in a healthy way most important.
Fire proofing be can inhibit or retardation burning and oneself be not easy to burning material.Its flame-retarding characteristic is main
The effect of flame retardant property and additive from material element.Phosphorus flame retardant is one of important type of fire retardant, it passes through
Two kinds of fire retardant mechanisms of gas phase and solid phase promote the flame retardant property of material.
There are two aspects for flame retardant property promotion of the hyperbranched fire retardant to material：First is the fire-retardant mode of condensed phase,
In can be divided into charcoal effect and coating effect again, phosphoric acid or acid anhydrides can be decomposed under phosphorus flame retardant high temperature, acid anhydrides can make
Material phosphorylated simultaneously discharges water outlet, and the material of phosphorylated can be changed into charcoal.The effect of fire retardant comes from this time：1. generating non-ignitable
Vapor；2. the protective effect of layer of charcoal；3. reducing combustible.P elements can also be such that the oxidable activated centre on carbon is passivated, shape
At inhibition graphitic carbon by oxygen free gas oxide coating.Second of fire retardant mechanism is that gas phase is fire-retardant, can be divided into chemical action and object
Reason acts on.Chemical action：In flame, fire retardant resolves into small molecule or free radical, they can make flame go hydroperoxyl radical dense
Degree reduces, to make fray-out of flame.Physical action：Gas phase flame retardant property is set to improve by heat of evaporation and specific heat capacity.
Diatomite is a kind of siliceous rock, is a kind of biogenic siliceous sedimentary rock, it is mainly by the something lost of ancient times diatom
The bones of the body are formed.Its chemical composition has certain flame retardant property based on silica.It is hyperbranched as dendrimer one
Kind, it is a kind of dendrimer of faulty symmetrical structure in structure, and have in structure tree-shaped big with perfection
The physicochemical property of molecule.Monomer polycondensation reaction generates soluble highly branched polymer, and this polymer is not perfect
Dendritic macromole, but the defective polymer of structure, this polymer are known as dissaving polymer.Dissaving polymer
Solution viscosity first increases with the increase of molecular weight, after be gradually reduced.
Largely studies have shown that the addition of phosphonium flame retardant can make the flame retardant property of material effectively improve.It is fire-retardant
The flame retardant property of agent is inversely proportional with its particle radius, and since grain size is smaller, intergranular active force is bigger, dispersion in the material
It is more difficult, it is therefore desirable to its molecular structure is designed, solution viscosity is reduced, improve the dispersion performance of fire retardant, make it easily
In being added in material.
Invention content
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide a kind of promotion dispersion performances
Hyperbranched phosphorous modification infusorial earth fire retardant and preparation method thereof.
The purpose of the present invention can be achieved through the following technical solutions：
A kind of hyperbranched phosphorous modification infusorial earth fire retardant, is prepared using the raw material of following parts by weight of component：
Natural rubber matrix：100, vulcanizing agent：2~3, accelerating agent：1~1.5, stearic acid：0.5~1.0, zinc oxide：3~
5, anti-aging agent：1~3, hyperbranched modification infusorial earth：10~15.
The hyperbranched modification infusorial earth is prepared using following methods：
(1) preparation of KH-560 modification infusorial earths
Under 40-60 DEG C of reaction temperature, absolute ethyl alcohol is added into the diatomite of drying, KH-560 is then added dropwise again,
It is washed using ethyl alcohol after suction filtration, obtained filter cake obtains KH-560 grafting diatomite through ultrasound, suction filtration, drying and processing；
(2) preparation of open loop modification infusorial earth
By diatomite, Co (Ac)2·4H2O、H2O and THF is being stirred for 24 hours in ice-water bath, is then warmed naturally to
Room temperature filters afterwards for 24 hours, is dried again using ethyl alcohol washing, obtains open loop modification infusorial earth；
(3) preparation of hyperbranched modification infusorial earth
By open loop modification infusorial earth, PER, [(the own ring -6- bases of 6- oxo -6H- dibenzo [c, e] [1,2] oxygen phospha) first
Base] succinic acid and thionyl chloride mix and dry, then poured out after reacting 2-4h in 100 DEG C of reflux water-dividings in oil bath pan, first
It is washed with massive laundering, extra carboxylic acid halides is become into carboxyl, is washed afterwards with a large amount of methanol, remove impurity；Obtain DDP- pentaerythrites
Hyperbranched modification infusorial earth.
The proportionate relationship of diatomite, absolute ethyl alcohol and KH-560 is 6~14g in step (1)：150~250mL：30~
The rate of addition of 50mL, KH-560 are 5~15mL/h.
Diatomite, Co (Ac) in step (2)2·4H2O、H2The proportionate relationship of O and THF is 6~14g：0.035~
0.071g：0.07~0.13mL：70~130mL
Open loop modification infusorial earth, PER and [(the own ring-of 6- oxo -6H- dibenzo [c, e] [1,2] oxygen phosphas in step (3)
6- yls) methyl] succinic acid proportionate relationship be 1g：0.25~0.35g：1.25~2.5g, open loop modification infusorial earth, PER, [(6-
Own ring -6- the bases of oxo -6H- dibenzo [c, e] [1,2] oxygen phospha) methyl] oxygen is added in succinic acid and thionyl chloride in water knockout drum
It is dry for during to change calcium.
The vulcanizing agent is sulphur.
The accelerating agent is 2- benzothiazolyl mercaptans,
The anti-aging agent is N- phenyl-2-naphthylamine class anti-aging agents.
The preparation method of hyperbranched phosphorous modification infusorial earth fire retardant prepares raw material, then successively by day by formula composition
T PNR matrix, zinc oxide, stearic acid, accelerating agent, anti-aging agent, hyperbranched modification infusorial earth and vulcanizing agent are thrown according to aforementioned proportion
Enter in open mill, be kneaded under conditions of temperature is 30~50 DEG C, that is, obtains the Flame-retardant natural rubber of the present invention.
Compared with prior art, the present invention is designed the molecular structure of fire retardant, so as to reduce solution viscosity,
The dispersion performance for improving fire retardant, makes it easier to be added in material.
The hydroxyl on itself and diatomite surface is reacted by hydrolyzing KH-560, is grafted to diatomite table by this technique
Face, then so that the terminal epoxy groups open loop of KH-560 is generated hydroxyl, the dicarboxylic acids base of excessive DDP by way of catalyst is added
Esterification occurs with the hydroxyl on KH-560 modification infusorial earths surface after group's chloride, is grafted to diatomite surface, is added simultaneously
Pentaerythrite and acyl chlorides and the diatomite that is grafted of acyl chlorides hyperbranched esterification occurs, finally plus water is former using hydroxyl displacement chlorine
Son is blocked.Because having been carried out to diatomite organically-modified, dispersibility is bad when solving the processing of single diatomite
Problem.And at the same time containing two kinds of silicon, phosphorus elements, the gentle mutually fire-retardant effect of solid phase is played when natural rubber burns, therefore
With good flame retardant property.
Specific implementation mode
With reference to specific embodiment, the present invention is described in detail.Following embodiment will be helpful to the technology of this field
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill of this field
For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention
Protection domain.
Comparative example 1
By natural rubber 100g, zinc oxide 3g, stearic acid 0.5g, accelerating agent 1g, anti-aging agent 1g and sulphur 2g etc. according to upper
It states in ratio input open mill, is kneaded under conditions of temperature is 30 DEG C, that is, obtains common natural rubber.
The fissipation factor of common natural flame retardant rubber, tensile strength, elongation at break, are shown in Table 2.
Comparative example 2
Natural rubber 100g, zinc oxide 4g, stearic acid 0.8g, accelerating agent 1.2g, anti-aging agent 2g and sulphur 2.5g etc. are pressed
It is put into open mill according to aforementioned proportion, is kneaded under conditions of temperature is 40 DEG C, that is, obtains common natural rubber.
The fissipation factor of common natural flame retardant rubber, tensile strength, elongation at break, are shown in Table 2.
Comparative example 3
By natural rubber 100g, zinc oxide 5g, stearic acid 1.0g, accelerating agent 1.5g, anti-aging agent 3g and sulphur 3g etc. according to
Aforementioned proportion is put into open mill, is kneaded under conditions of temperature is 50 DEG C, that is, obtains common natural rubber.
The fissipation factor of common natural flame retardant rubber, tensile strength, elongation at break, are shown in Table 2.
Embodiment 1
The diatomite of 14g drying is added in three-necked flask, 200mL absolute ethyl alcohols are added, constant pressure point is used in 6 hours
30mL KH-560 are added into flask with the rate of 5mL/h for liquid funnel, and reaction temperature is 50 DEG C.It filters, is washed using ethyl alcohol,
Filter cake is transferred to conical flask ultrasound 20min, is filtered, drying obtains KH-560 grafting diatomite.10g is added in conical flask
Diatomite, 0.053g Co (Ac)2·4H2O, 0.1mL H2O and 100mL THF, are put into magneton, are stirred in ice-water bath for 24 hours, from
It so is warming up to room temperature, does not during which have to add ice.It filters after 24 hours, is washed using 50% ethanol water, be put into baking oven baking
It is dry, obtain open loop KH-560 modification infusorial earths.35g DDP, the pentaerythrite of 5g and the organically-modified diatomite of 20g are weighed in three necks
In flask, excessive thionyl chloride is added as acylating agent and solvent, is stirred 4 hours in 100 DEG C.Then it filters, is washed using methanol
It washs, is dried in vacuo 4 hours, obtain the fire retardant of the present invention, obtain hyperbranched modification infusorial earth.By natural rubber 100g, oxidation
Zinc 3g, stearic acid 0.5g, accelerating agent 1g, anti-aging agent 1g, hyperbranched modified organic silicon diatomaceous earth 20g and sulphur 2g etc. are according to above-mentioned ratio
In example input open mill, it is kneaded under conditions of temperature is 30 DEG C, that is, obtains the Flame-retardant natural rubber of the present invention.
The particle size of hyperbranched modified organic silicon diatomaceous earth is shown in Table 1.
The limit oxygen index of Flame-retardant natural rubber, level-vertical combustion time, heat release rate, are shown in Table 2.
Embodiment 2
The diatomite of 6g drying is added in three-necked flask, 150mL absolute ethyl alcohols are added, constant pressure point is used in 4 hours
60mL KH-560 are added into flask with the rate of 10mL/h for liquid funnel, and reaction temperature is 60 DEG C.It filters, is washed using ethyl alcohol,
Filter cake is transferred to conical flask ultrasound 20min, is filtered, drying obtains KH-560 grafting diatomite.14g is added in conical flask
Diatomite, 0.035g Co (Ac)2·4H2O, 0.07mL H2O and 130mL THF, are put into magneton, are stirred in ice-water bath for 24 hours,
Room temperature is warmed naturally to, does not during which have to add ice.It is filtered after 24 hours, is washed using 50% ethanol water, be put into baking oven
Drying, obtains open loop KH-560 modification infusorial earths.25g DDP, the pentaerythrite of 6g and the organically-modified diatomite of 20g are weighed in three
In neck flask, excessive thionyl chloride is added as acylating agent and solvent, is stirred 3 hours in 120 DEG C.Then it filters, uses methanol
Washing is dried in vacuo 4 hours, is obtained the fire retardant of the present invention, is obtained hyperbranched modification infusorial earth.By natural rubber 100g, oxygen
Change zinc 4g, stearic acid 0.8g, accelerating agent 1.2g, anti-aging agent 2g, hyperbranched modified organic silicon diatomaceous earth 20g and sulphur 2.5g etc. according to
Aforementioned proportion is put into open mill, is kneaded under conditions of temperature is 30 DEG C, that is, obtains the Flame-retardant natural rubber of the present invention.
The particle size of hyperbranched modified organic silicon diatomaceous earth is shown in Table 1.
The limit oxygen index of Flame-retardant natural rubber, level-vertical combustion time, heat release rate, are shown in Table 2.
Embodiment 3
The diatomite of 10g drying is added in three-necked flask, 250mL absolute ethyl alcohols are added, constant pressure point is used in 8 hours
90mL KH-560 are added into flask with the rate of 15mL/h for liquid funnel, and reaction temperature is 60 DEG C.It filters, is washed using ethyl alcohol,
Filter cake is transferred to conical flask ultrasound 20min, is filtered, drying obtains KH-560 grafting diatomite.6g silicon is added in conical flask
Diatomaceous earth, 0.071g Co (Ac) 24H2O, 0.13mL H2O and 70mLTHF, is put into magneton, is stirred in ice-water bath for 24 hours, natural
It is warming up to room temperature, does not during which have to add ice.It filters after 24 hours, is washed using 50% ethyl alcohol, be put into baking oven drying, opened
Ring KH-560 modification infusorial earths.50g DDP, the pentaerythrite of 7g and the organically-modified diatomite of 20g are weighed in three-neck flask, is added
Enter excessive thionyl chloride as acylating agent and solvent, is stirred 4 hours in 90 DEG C.Then it filters, is washed using methanol, is dried in vacuo
4 hours, the fire retardant of the present invention is obtained, hyperbranched modification infusorial earth is obtained.By natural rubber 100g, zinc oxide 5g, stearic acid
1g, accelerating agent 1.5g, anti-aging agent 3g, hyperbranched modified organic silicon diatomaceous earth 20g and sulphur 3g etc. put into mill according to aforementioned proportion
It in machine, is kneaded under conditions of temperature is 30 DEG C, that is, obtains the Flame-retardant natural rubber of the present invention.
The particle size of hyperbranched modified organic silicon diatomaceous earth is shown in Table 1.
The limit oxygen index of Flame-retardant natural rubber, level-vertical combustion time, heat release rate, are shown in Table 2.
The particle size of 1 modified organic silicon diatomaceous earth of table
| Embodiment | Grain size (mm) |
| 1 | 2.6 |
| 2 | 2.2 |
| 3 | 2.5 |
The limit oxygen index of 2 Flame-retardant natural rubber of table, horizontal firing time, vertical combustion time
The infrared peak position of dominant spectral of 3 hyperbranched fire retardant of table and its corresponding group
Embodiment 4
A kind of hyperbranched phosphorous modification infusorial earth fire retardant, is prepared using the raw material of following parts by weight of component：Naturally
Rubber matrix：100, sulphur：2, accelerating agent 2- benzothiazolyl mercaptans：1, stearic acid：0.5, zinc oxide：3, N- phenyl -2- naphthalenes
Amines antioxidants：1, hyperbranched modification infusorial earth：10.
Wherein hyperbranched modification infusorial earth is prepared using following methods：
(1) preparation of KH-560 modification infusorial earths
Under 40 DEG C of reaction temperature, 150mL absolute ethyl alcohols are added in the diatomite dried to 14g, are then added dropwise again
The rate of addition of the KH-560 of 30mL, KH-560 are 5mL/h, are washed using ethyl alcohol after suction filtration, and obtained filter cake is through ultrasound, pumping
Filter, drying and processing obtain KH-560 grafting diatomite；
(2) preparation of open loop modification infusorial earth
By 6g diatomite, the Co (Ac) of 0.035g2·4H2O, the H of 0.07mL2The THF of O and 70mL is being stirred in ice-water bath
It mixes mixing for 24 hours, then warms naturally to room temperature, filter afterwards for 24 hours, dried again using ethyl alcohol washing, obtain open loop modification infusorial earth；
(3) preparation of hyperbranched modification infusorial earth
By 1g open loops modification infusorial earth, PER, 1.25g [(6- oxo -6H- dibenzo [c, e] [1,2] oxygen phospha of 0.25g
Own ring -6- bases) methyl] succinic acid and thionyl chloride mix and dry, then in 100 DEG C of reflux water-dividings, reaction in oil bath pan
It pours out after 2h, is first washed with massive laundering, extra carboxylic acid halides is become into carboxyl, is washed afterwards with a large amount of methanol, remove impurity, obtain
The hyperbranched modification infusorial earth of DDP- pentaerythrites.
Hyperbranched phosphorous modification infusorial earth fire retardant prepares raw material in the preparation, by formula composition, then successively will be natural
Rubber matrix, zinc oxide, stearic acid, accelerating agent, anti-aging agent, hyperbranched modification infusorial earth and sulphur agent are put into according to aforementioned proportion
It in open mill, is kneaded under conditions of temperature is 30 DEG C, that is, obtains the Flame-retardant natural rubber of the present invention.
Embodiment 5
A kind of hyperbranched phosphorous modification infusorial earth fire retardant, is prepared using the raw material of following parts by weight of component：Naturally
Rubber matrix：100, sulphur：3, accelerating agent 2- benzothiazolyl mercaptans：1.5, stearic acid：1.0, zinc oxide：5, N- phenyl -2-
Naphthylamine antioxidant：3, hyperbranched modification infusorial earth：15.
Wherein hyperbranched modification infusorial earth is prepared using following methods：
(1) preparation of KH-560 modification infusorial earths
Under 40 DEG C of reaction temperature, 250mL absolute ethyl alcohols are added in the diatomite dried to 6g, 50mL is then added dropwise again
KH-560, the rate of addition of KH-560 is 15mL/h, is washed using ethyl alcohol after suction filtration, obtained filter cake through ultrasound, filter, dry
Dry-cure obtains KH-560 grafting diatomite；
(2) preparation of open loop modification infusorial earth
By 14g diatomite, the Co (Ac) of 0.071g2·4H2O, the H of 0.13mL2The THF of O and 130mL is in ice-water bath
It is stirred for 24 hours, then warms naturally to room temperature, filter afterwards for 24 hours, dried again using ethyl alcohol washing, obtain open loop and be modified diatom
Soil；
(3) preparation of hyperbranched modification infusorial earth
By 1g open loops modification infusorial earth, PER, 2.5g [(6- oxo -6H- dibenzo [c, e] [1,2] oxygen phospha of 0.35g
Own ring -6- bases) methyl] succinic acid and thionyl chloride mix and dry, then in 100 DEG C of reflux water-dividings, reaction in oil bath pan
It pours out after 4h, is first washed with massive laundering, extra carboxylic acid halides is become into carboxyl, is washed afterwards with a large amount of methanol, remove impurity, obtain
The hyperbranched modification infusorial earth of DDP- pentaerythrites.
Hyperbranched phosphorous modification infusorial earth fire retardant prepares raw material in the preparation, by formula composition, then successively will be natural
Rubber matrix, zinc oxide, stearic acid, accelerating agent, anti-aging agent, hyperbranched modification infusorial earth and sulphur agent are put into according to aforementioned proportion
It in open mill, is kneaded under conditions of temperature is 50 DEG C, that is, obtains the Flame-retardant natural rubber of the present invention.
Specific embodiments of the present invention are described above.It is to be appreciated that the invention is not limited in above-mentioned
Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow
Ring the substantive content of the present invention.
Claims (9)
1. a kind of hyperbranched phosphorous modification infusorial earth fire retardant, which is characterized in that the fire retardant is using following parts by weight of component
Raw material is prepared：
Natural rubber matrix：100, vulcanizing agent：2~3, accelerating agent：1~1.5, stearic acid：0.5~1.0, zinc oxide：3~5, prevent
Old agent：1~3, hyperbranched modification infusorial earth：10~15；
The hyperbranched modification infusorial earth is prepared using following methods：
(1) preparation of KH-560 modification infusorial earths
Under 40-60 DEG C of reaction temperature, absolute ethyl alcohol is added into the diatomite of drying, KH-560 is then added dropwise again, filters
It is washed afterwards using ethyl alcohol, obtained filter cake obtains KH-560 grafting diatomite through ultrasound, suction filtration, drying and processing；
(2) preparation of open loop modification infusorial earth
KH-560 is grafted diatomite, Co (Ac)2·4H2O、H2O and THF is stirred for 24 hours in ice-water bath, is then risen naturally
It warms to room temperature, filters afterwards for 24 hours, dried again using ethyl alcohol washing, obtain open loop modification infusorial earth；
(3) preparation of hyperbranched modification infusorial earth
By open loop modification infusorial earth, pentaerythrite, [(the own ring -6- bases of 6- oxo -6H- dibenzo [c, e] [1,2] oxygen phospha) first
Base] succinic acid and thionyl chloride mix and dry, then poured out after reacting 2-4h in 100 DEG C of reflux water-dividings in oil bath pan, first
It is washed with massive laundering, extra carboxylic acid halides is become into carboxyl, is washed afterwards with a large amount of methanol, remove impurity；Obtain DDP- pentaerythrites
Hyperbranched modification infusorial earth.
2. the hyperbranched phosphorous modification infusorial earth fire retardant of one kind according to claim 1, which is characterized in that in step (1)
The proportionate relationship of diatomite, absolute ethyl alcohol and KH-560 is 6~14g：150~250mL：The dropwise addition speed of 30~50mL, KH-560
Degree is 20~60mL/6h.
3. the hyperbranched phosphorous modification infusorial earth fire retardant of one kind according to claim 1, which is characterized in that in step (2)
KH-560 is grafted diatomite, Co (Ac)2·4H2O、H2The proportionate relationship of O and THF is 6~14g：0.035~0.071g：0.07~
0.13mL：70~130mL.
4. the hyperbranched phosphorous modification infusorial earth fire retardant of one kind according to claim 1, which is characterized in that in step (3)
Open loop modification infusorial earth, pentaerythrite, [(the own ring -6- bases of 6- oxo -6H- dibenzo [c, e] [1,2] oxygen phospha) methyl] fourth two
The proportionate relationship of acid and thionyl chloride is 1.4~2.6g：0.816~2.176g：5.544~8.316g：15~35mL.
5. the hyperbranched phosphorous modification infusorial earth fire retardant of one kind according to claim 1, which is characterized in that in step (3)
Open loop modification infusorial earth, pentaerythrite, [(the own ring -6- bases of 6- oxo -6H- dibenzo [c, e] [1,2] oxygen phospha) methyl] fourth two
Calcium oxide is added in water knockout drum and is dried for during for acid and thionyl chloride.
6. the hyperbranched phosphorous modification infusorial earth fire retardant of one kind according to claim 1, which is characterized in that the vulcanization
Agent is sulphur.
7. the hyperbranched phosphorous modification infusorial earth fire retardant of one kind according to claim 1, which is characterized in that the promotion
Agent is 2- benzothiazolyl mercaptans.
8. the hyperbranched phosphorous modification infusorial earth fire retardant of one kind according to claim 1, which is characterized in that described is anti-old
Agent is N- phenyl-2-naphthylamine class anti-aging agents.
9. the preparation method of hyperbranched phosphorous modification infusorial earth fire retardant as described in claim 1, which is characterized in that by formula
Composition prepares raw material, then successively by natural rubber matrix, zinc oxide, stearic acid, accelerating agent, antioxidant D, hyperbranched modified silicon
Diatomaceous earth and vulcanizing agent are put into according to aforementioned proportion in open mill, are kneaded, that is, obtained under conditions of temperature is 30~50 DEG C
Hyperbranched phosphorous modification infusorial earth fire retardant.
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| CN115594978B (en) * | 2022-10-29 | 2024-03-05 | 江苏加富新材料科技有限公司 | High-voltage-resistant insulating rubber plate and preparation method thereof |
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