CN107603068A - A kind of polyvinyl chloride carbonized agent and preparation method thereof - Google Patents
A kind of polyvinyl chloride carbonized agent and preparation method thereof Download PDFInfo
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- CN107603068A CN107603068A CN201710947384.1A CN201710947384A CN107603068A CN 107603068 A CN107603068 A CN 107603068A CN 201710947384 A CN201710947384 A CN 201710947384A CN 107603068 A CN107603068 A CN 107603068A
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Abstract
The invention is related to a kind of polyvinyl chloride carbonized agent, including following raw material components：Ammonium silicate modified polyvinyl chloride, zeolite molecular sieve, urea oxalate, silica gel improved silica aeroge, stannous pyrophosphate, ferric stearate, ammonium silicate modified polyvinyl chloride is by polyvinyl chloride, ammonium silicate, neopelex, OP10 and polyformaldehyde reaction are made, zeolite molecular sieve is by zeolite powder, sodium metasilicate, calcium dihydrogen phosphate, phenolic resin and cupric oxide reaction are made, urea oxalate is by ammonium oxalate, urea hydrochloride, isopropanol and ethanol synthesis are made, silica gel improved silica aeroge is by silica gel, tetraethyl orthosilicate, sodium metasilicate, dodecyl sodium sulfate, water and ethanol synthesis are made.The invention has excellent charing performance.
Description
Technical field
The invention is related to a kind of polyvinyl chloride carbonized agent and preparation method thereof.
Background technology
Polyvinyl chloride is one of five big thermoplastic synthetic resins, has corrosion-resistant, insulation, fire-retardant, easy processing shaping, high machine
The advantages such as tool intensity, polyvinyl chloride are widely used in agricultural, communications and transportation, film, packaging, pipeline, communications and transportation, electric wire electricity
The fields such as cable.
At present, pvc material needs further lifting in charing performance.The invention uses ammonium silicate modified polyvinyl chloride
Alkene, zeolite molecular sieve, urea oxalate, silica gel improved silica aeroge, stannous pyrophosphate are prepared for polyvinyl chloride carbonized agent, should
Polyvinyl chloride carbonized agent prepared by method has excellent charing performance.
The content of the invention
The purpose of the invention is to provide a kind of preparation method of polyvinyl chloride carbonized agent, and this method is by changing reactant
Raw material and technology mode, the material of preparation have excellent charing performance.
To achieve these goals, the technical scheme of the invention is as follows.
A kind of polyvinyl chloride carbonized agent and preparation method thereof, specifically includes following steps：(1), by silica gel, silicic acid tetrem
Ester, sodium metasilicate, dodecyl sodium sulfate, water and ethanol are 5 according to quality parts ratio：45~63：39~56：7~13：64~
80：123~140 are added in hydrothermal reaction kettle, and 6~13h, product warp are reacted under the conditions of 168~185 DEG C of maintenance system temperature
1000mL water washings 3 times, 1000mL ethanol wash 3 times, 55 DEG C, -0.09MPa vacuum drying 18min, obtain silica gel and are modified dioxy
SiClx aeroge；(2), by ammonium oxalate, urea hydrochloride, isopropanol and ethanol according to quality parts ratio 40：11~21：59~71：58
~70 are added in reactor, and mixing speed is 97~117r/min, 93~100 DEG C of maintenance system temperature, -0.04MPa conditions
0.5~1h of lower reaction, product are evaporated under reduced pressure 0.5h through 100 DEG C, -0.05MPa, obtain urea oxalate；(3), by zeolite powder, silicic acid
Sodium, calcium dihydrogen phosphate, phenolic resin and cupric oxide are according to quality parts ratio 60：8~17：10~21：16~27：5~12 add
Into ball mill, drum speed is 30~36r/min, and 0.5h, product warp are reacted under the conditions of 35~51 DEG C of maintenance system temperature
200 DEG C of roasting 2h, 300 DEG C of roasting 2h, 400 DEG C of roasting 2h, 500 DEG C of roasting 2h, 600 DEG C of roasting 2h, 700 DEG C of roasting 3h, are produced
To zeolite molecular sieve；(4), by polyvinyl chloride, ammonium silicate, neopelex, OP10 and polyformaldehyde according to mass fraction
Than 60：35~52：9~18：7~14：12~20 are added in high-speed mixer, mixing velocity 900r/min, maintenance system
2~7min is reacted under the conditions of 173 DEG C of temperature, with extruder in 175 DEG C of extruding pelletizations of temperature, that is, ammonium silicate is obtained and is modified polychlorostyrene
Ethene；(5), by ammonium silicate modified polyvinyl chloride, zeolite molecular sieve, urea oxalate, silica gel improved silica aeroge, pyrophosphoric acid
Stannous, ferric stearate are according to quality parts ratio 70：19~32：34~46：29~45：13~25：2~7 are added to mixed at high speed
In machine, with high-speed mixer in 175 DEG C of temperature, 950 r/min 3~8min of hybrid reaction, with extruder in temperature 174~185
DEG C extruding pelletization, that is, obtain polyvinyl chloride carbonized agent.
The preparation method of polyvinyl chloride carbonized agent described in the invention, comprises the following steps：
(1) it is, 5 according to quality parts ratio by silica gel, tetraethyl orthosilicate, sodium metasilicate, dodecyl sodium sulfate, water and ethanol：45
~63：39~56：7~13：64~80：123~140 are added in hydrothermal reaction kettle, 168~185 DEG C of bars of maintenance system temperature
6~13h is reacted under part, product washs 3 times through 1000mL water washings 3 times, 1000mL ethanol, 55 DEG C, -0.09MPa vacuum drying
18min, obtain silica gel improved silica aeroge；The purpose of described dodecyl sodium sulfate is in order to improve silica gas
The porosity of gel.
(2), by ammonium oxalate, urea hydrochloride, isopropanol and ethanol according to quality parts ratio 40：11~21：59~71：58~70
It is added in reactor, mixing speed is 97~117r/min, anti-under the conditions of 93~100 DEG C of maintenance system temperature, -0.04MPa
0.5~1h is answered, product is evaporated under reduced pressure 0.5h through 100 DEG C, -0.05MPa, obtains urea oxalate；Described isopropanol and the mesh of ethanol
In order to improve reaction rate.
(3), by zeolite powder, sodium metasilicate, calcium dihydrogen phosphate, phenolic resin and cupric oxide according to quality parts ratio 60：8~
17：10~21：16~27：5~12 are added in ball mill, and drum speed is 30~36r/min, maintenance system temperature 35~51
React 0.5h under the conditions of DEG C, product is through 200 DEG C of roasting 2h, 300 DEG C of roasting 2h, 400 DEG C of roasting 2h, 500 DEG C of roasting 2h, 600 DEG C
2h is calcined, 700 DEG C of roasting 3h, that is, obtains zeolite molecular sieve；Described sodium metasilicate, calcium dihydrogen phosphate, phenolic resin and cupric oxide
Purpose in order to improve the mechanical strength of molecular sieve.
(4), by polyvinyl chloride, ammonium silicate, neopelex, OP10 and polyformaldehyde according to quality parts ratio 60：
35~52：9~18：7~14：12~20 are added in high-speed mixer, mixing velocity 900r/min, maintenance system temperature
2~7min is reacted under the conditions of 173 DEG C, with extruder in 175 DEG C of extruding pelletizations of temperature, that is, obtains ammonium silicate modified polyvinyl chloride；
The purpose of described ammonium silicate in order to reduce polyvinyl chloride surface oxygen content and improve polyvinyl chloride into charcoal.
(5), by ammonium silicate modified polyvinyl chloride, zeolite molecular sieve, urea oxalate, silica gel improved silica aeroge, Jiao
Phosphoric acid stannous chloride, ferric stearate are according to quality parts ratio 70：19~32：34~46：29~45：13~25：2~7 are added at a high speed
In mixer, with high-speed mixer in 175 DEG C of temperature, 950 r/min 3~8min of hybrid reaction, with extruder temperature 174~
185 DEG C of extruding pelletizations, that is, obtain polyvinyl chloride carbonized agent；The purpose of described stannous pyrophosphate is in order to reduce polyvinyl chloride surface
Oxygen content.
The beneficial effect of the invention is：
1st, tetraethyl orthosilicate and sodium metasilicate can be hydrolyzed to silicic acid in hydrothermal reaction kettle, and dodecyl sodium sulfate has in aqueous phase
Excellent frothing capacity, the porosity of silicic acid and aerosil, the silica gel improved silica gas of preparation can be improved
Gel can substantially reduce polyvinyl chloride surface oxygen content when polyvinyl chloride burns, so as to improve the charing performance of polyvinyl chloride；
2nd, the chloride binding in the ammonium ion and urea hydrochloride in ammonium oxalate, volatile ammonium chloride can be generated and with ethanol and different
Propyl alcohol departs from reaction system, generates urea oxalate, and urea oxalate can resolve into inertia when polyvinyl chloride burns in polyvinyl chloride surface
Gas, so as to reduce polyvinyl chloride surface oxygen content, improve polyvinyl chloride into charcoal；
3rd, sodium metasilicate, calcium dihydrogen phosphate and cupric oxide can improve the heat resistance and mechanics of zeolite molecular sieve as inorganic bond
Intensity；Phenolic resin can improve the processing forming and cryomechanics intensity of zeolite molecular sieve, and zeolite molecular sieve can prevent oxygen
In the enrichment of polyvinyl chloride surface, so as to improve polyvinyl chloride into charcoal；
4th, when polyvinyl chloride burns, polyformaldehyde can consume the oxygen of polyvinyl chloride surface, reduce polyvinyl chloride surface oxygen content
While, ammonium silicate is produced inert gas by thermal decomposition, polyvinyl chloride surface oxygen content is further reduced, so as to improve polychlorostyrene second
Alkene into charcoal；
5th, stannous pyrophosphate has reproducibility, can reduce polyvinyl chloride surface oxygen content, so as to improve polyvinyl chloride into charcoal；
In ammonium silicate modified polyvinyl chloride, zeolite molecular sieve, urea oxalate, silica gel improved silica aeroge, stannous pyrophosphate collaboration
Under effect, it is excellent into charcoal to assign polyvinyl chloride.
Embodiment
The embodiment of the invention is described with reference to embodiment, to be better understood from the invention.
Embodiment 1
A kind of polyvinyl chloride carbonized agent, its preparation method comprise the following steps：
(1) 5 parts of silica gel, 53 parts of tetraethyl orthosilicates, 44 parts of sodium metasilicate, 8 parts of dodecyl sodium sulfates, 75 parts of water and 130 parts, are weighed
Ethanol is added in hydrothermal reaction kettle, reacts 8h under the conditions of 175 DEG C of maintenance system temperature, product through 1000mL water washings 3 times,
1000mL ethanol washs 3 times, 55 DEG C, -0.09MPa vacuum drying 18min, obtains silica gel improved silica aeroge；
(2), weigh 40 parts of ammonium oxalate, 16 parts of urea hydrochlorides, 65 parts of isopropanols and 62 parts of ethanol to be added in reactor, mixing speed
For 100r/min, 0.6h is reacted under the conditions of 96 DEG C of maintenance system temperature, -0.04MPa, product depressurizes through 100 DEG C, -0.05MPa
0.5h is distilled, obtains urea oxalate；
(3) 60 parts of zeolite powders, 10 parts of sodium metasilicate, 14 parts of calcium dihydrogen phosphates, 21 parts of phenolic resin and 7 parts of cupric oxide, are weighed to add
Into ball mill, drum speed 33r/min, 0.5h is reacted under the conditions of 40 DEG C of maintenance system temperature, product is through 200 DEG C of roastings
2h, 300 DEG C of roasting 2h, 400 DEG C of roasting 2h, 500 DEG C of roasting 2h, 600 DEG C of roasting 2h, 700 DEG C of roasting 3h, that is, obtains zeolite molecules
Sieve；
(4) 60 parts of polyvinyl chloride, 40 parts of ammonium silicates, 10 parts of neopelexes, 9 parts of OP10 and 15 part of polyformaldehyde, are weighed
It is added in high-speed mixer, mixing velocity 900r/min, 3min is reacted under the conditions of 173 DEG C of maintenance system temperature, with extrusion
Machine obtains ammonium silicate modified polyvinyl chloride in 175 DEG C of extruding pelletizations of temperature；
(5) 70 parts of ammonium silicate modified polyvinyl chlorides, 23 parts of zeolite molecular sieves, 39 parts of urea oxalates, 41 parts of silica gel, are weighed and are modified dioxy
SiClx aeroge, 20 parts of stannous pyrophosphates, 4 parts of ferric stearates are added in high-speed mixer, with high-speed mixer in temperature 175
DEG C, 950 r/min hybrid reaction 3min, with extruder in 176 DEG C of extruding pelletizations of temperature, that is, obtain polyvinyl chloride carbonized agent.
Embodiment 2
A kind of polyvinyl chloride carbonized agent, its preparation method comprise the following steps：
(1) 5 parts of silica gel, 45 parts of tetraethyl orthosilicates, 39 parts of sodium metasilicate, 7 parts of dodecyl sodium sulfates, 64 parts of water and 123 parts, are weighed
Ethanol is added in hydrothermal reaction kettle, reacts 13h under the conditions of 168 DEG C of maintenance system temperature, product through 1000mL water washings 3 times,
1000mL ethanol washs 3 times, 55 DEG C, -0.09MPa vacuum drying 18min, obtains silica gel improved silica aeroge；
(2), weigh 40 parts of ammonium oxalate, 11 parts of urea hydrochlorides, 59 parts of isopropanols and 58 parts of ethanol to be added in reactor, mixing speed
For 97r/min, 1h is reacted under the conditions of 93 DEG C of maintenance system temperature, -0.04MPa, product is evaporated under reduced pressure through 100 DEG C, -0.05MPa
0.5h, obtain urea oxalate；
(3) 60 parts of zeolite powders, 8 parts of sodium metasilicate, 10 parts of calcium dihydrogen phosphates, 16 parts of phenolic resin and 5 parts of cupric oxide, are weighed to be added to
In ball mill, drum speed 30r/min reacts 0.5h under the conditions of 35 DEG C of maintenance system temperature, product through 200 DEG C of roasting 2h,
300 DEG C of roasting 2h, 400 DEG C of roasting 2h, 500 DEG C of roasting 2h, 600 DEG C of roasting 2h, 700 DEG C of roasting 3h, that is, obtain zeolite molecular sieve；
(4) 60 parts of polyvinyl chloride, 35 parts of ammonium silicates, 9 parts of neopelexes, 7 parts of OP10 and 12 part of polyformaldehyde, are weighed to add
Enter into high-speed mixer, mixing velocity 900r/min, react 2min under the conditions of 173 DEG C of maintenance system temperature, use extruder
In 175 DEG C of extruding pelletizations of temperature, that is, obtain ammonium silicate modified polyvinyl chloride；
(5) 70 parts of ammonium silicate modified polyvinyl chlorides, 19 parts of zeolite molecular sieves, 34 parts of urea oxalates, 29 parts of silica gel, are weighed and are modified dioxy
SiClx aeroge, 13 parts of stannous pyrophosphates, 2 parts of ferric stearates are added in high-speed mixer, with high-speed mixer in temperature 175
DEG C, 950 r/min hybrid reaction 3min, with extruder in 174 DEG C of extruding pelletizations of temperature, that is, obtain polyvinyl chloride carbonized agent.
Embodiment 3
A kind of polyvinyl chloride carbonized agent, its preparation method comprise the following steps：
(1) 5 parts of silica gel, 63 parts of tetraethyl orthosilicates, 56 parts of sodium metasilicate, 13 parts of dodecyl sodium sulfates, 80 parts of water and 140, are weighed
Part ethanol is added in hydrothermal reaction kettle, 6h is reacted under the conditions of 185 DEG C of maintenance system temperature, product is through 1000mL water washings 3
Secondary, 1000mL ethanol washs 3 times, 55 DEG C, -0.09MPa vacuum drying 18min, obtains silica gel improved silica aeroge；
(2), weigh 40 parts of ammonium oxalate, 21 parts of urea hydrochlorides, 71 parts of isopropanols and 70 parts of ethanol to be added in reactor, mixing speed
For 117r/min, 0.5h is reacted under the conditions of 100 DEG C of maintenance system temperature, -0.04MPa, product depressurizes through 100 DEG C, -0.05MPa
0.5h is distilled, obtains urea oxalate；
(3) 60 parts of zeolite powders, 17 parts of sodium metasilicate, 21 parts of calcium dihydrogen phosphates, 27 parts of phenolic resin and 12 parts of cupric oxide, are weighed to add
Into ball mill, drum speed 36r/min, 0.5h is reacted under the conditions of 51 DEG C of maintenance system temperature, product is through 200 DEG C of roastings
2h, 300 DEG C of roasting 2h, 400 DEG C of roasting 2h, 500 DEG C of roasting 2h, 600 DEG C of roasting 2h, 700 DEG C of roasting 3h, that is, obtains zeolite molecules
Sieve；
(4) 60 parts of polyvinyl chloride, 52 parts of ammonium silicates, 18 parts of neopelexes, 14 parts of OP10 and 20 part of polyformaldehyde, are weighed
It is added in high-speed mixer, mixing velocity 900r/min, 7min is reacted under the conditions of 173 DEG C of maintenance system temperature, with extrusion
Machine obtains ammonium silicate modified polyvinyl chloride in 175 DEG C of extruding pelletizations of temperature；
(5) 70 parts of ammonium silicate modified polyvinyl chlorides, 32 parts of zeolite molecular sieves, 46 parts of urea oxalates, 45 parts of silica gel, are weighed and are modified dioxy
SiClx aeroge, 25 parts of stannous pyrophosphates, 7 parts of ferric stearates are added in high-speed mixer, with high-speed mixer in temperature 175
DEG C, 950 r/min hybrid reaction 8min, with extruder in 185 DEG C of extruding pelletizations of temperature, that is, obtain polyvinyl chloride carbonized agent.
Embodiment 4
A kind of polyvinyl chloride carbonized agent, its preparation method comprise the following steps：
(1) 5 parts of silica gel, 50 parts of tetraethyl orthosilicates, 40 parts of sodium metasilicate, 10 parts of dodecyl sodium sulfates, 70 parts of water and 125, are weighed
Part ethanol is added in hydrothermal reaction kettle, 7h is reacted under the conditions of 170 DEG C of maintenance system temperature, product is through 1000mL water washings 3
Secondary, 1000mL ethanol washs 3 times, 55 DEG C, -0.09MPa vacuum drying 18min, obtains silica gel improved silica aeroge；
(2), weigh 40 parts of ammonium oxalate, 16 parts of urea hydrochlorides, 61 parts of isopropanols and 63 parts of ethanol to be added in reactor, mixing speed
For 103r/min, 0.7h is reacted under the conditions of 96 DEG C of maintenance system temperature, -0.04MPa, product depressurizes through 100 DEG C, -0.05MPa
0.5h is distilled, obtains urea oxalate；
(3) 60 parts of zeolite powders, 9 parts of sodium metasilicate, 12 parts of calcium dihydrogen phosphates, 17 parts of phenolic resin and 11 parts of cupric oxide, are weighed to add
Into ball mill, drum speed 31r/min, 0.5h is reacted under the conditions of 39 DEG C of maintenance system temperature, product is through 200 DEG C of roastings
2h, 300 DEG C of roasting 2h, 400 DEG C of roasting 2h, 500 DEG C of roasting 2h, 600 DEG C of roasting 2h, 700 DEG C of roasting 3h, that is, obtains zeolite molecules
Sieve；
(4) 60 parts of polyvinyl chloride, 38 parts of ammonium silicates, 17 parts of neopelexes, 8 parts of OP10 and 13 part of polyformaldehyde, are weighed
It is added in high-speed mixer, mixing velocity 900r/min, 6min is reacted under the conditions of 173 DEG C of maintenance system temperature, with extrusion
Machine obtains ammonium silicate modified polyvinyl chloride in 175 DEG C of extruding pelletizations of temperature；
(5) 70 parts of ammonium silicate modified polyvinyl chlorides, 21 parts of zeolite molecular sieves, 36 parts of urea oxalates, 43 parts of silica gel, are weighed and are modified dioxy
SiClx aeroge, 14 parts of stannous pyrophosphates, 5 parts of ferric stearates are added in high-speed mixer, with high-speed mixer in temperature 175
DEG C, 950 r/min hybrid reaction 6min, with extruder in 177 DEG C of extruding pelletizations of temperature, that is, obtain polyvinyl chloride carbonized agent.
Embodiment 5
A kind of polyvinyl chloride carbonized agent, its preparation method comprise the following steps：
(1) 5 parts of silica gel, 53 parts of tetraethyl orthosilicates, 44 parts of sodium metasilicate, 11 parts of dodecyl sodium sulfates, 71 parts of water and 128, are weighed
Part ethanol is added in hydrothermal reaction kettle, 7h is reacted under the conditions of 173 DEG C of maintenance system temperature, product is through 1000mL water washings 3
Secondary, 1000mL ethanol washs 3 times, 55 DEG C, -0.09MPa vacuum drying 18min, obtains silica gel improved silica aeroge；
(2), weigh 40 parts of ammonium oxalate, 13 parts of urea hydrochlorides, 62 parts of isopropanols and 66 parts of ethanol to be added in reactor, mixing speed
For 115r/min, 0.8h is reacted under the conditions of 99 DEG C of maintenance system temperature, -0.04MPa, product depressurizes through 100 DEG C, -0.05MPa
0.5h is distilled, obtains urea oxalate；
(3) 60 parts of zeolite powders, 16 parts of sodium metasilicate, 20 parts of calcium dihydrogen phosphates, 25 parts of phenolic resin and 11 parts of cupric oxide, are weighed to add
Into ball mill, drum speed 33r/min, 0.5h is reacted under the conditions of 50 DEG C of maintenance system temperature, product is through 200 DEG C of roastings
2h, 300 DEG C of roasting 2h, 400 DEG C of roasting 2h, 500 DEG C of roasting 2h, 600 DEG C of roasting 2h, 700 DEG C of roasting 3h, that is, obtains zeolite molecules
Sieve；
(4) 60 parts of polyvinyl chloride, 51 parts of ammonium silicates, 16 parts of neopelexes, 11 parts of OP10 and 17 part of polyformaldehyde, are weighed
It is added in high-speed mixer, mixing velocity 900r/min, 4min is reacted under the conditions of 173 DEG C of maintenance system temperature, with extrusion
Machine obtains ammonium silicate modified polyvinyl chloride in 175 DEG C of extruding pelletizations of temperature；
(5) 70 parts of ammonium silicate modified polyvinyl chlorides, 31 parts of zeolite molecular sieves, 41 parts of urea oxalates, 40 parts of silica gel, are weighed and are modified dioxy
SiClx aeroge, 22 parts of stannous pyrophosphates, 3 parts of ferric stearates are added in high-speed mixer, with high-speed mixer in temperature 175
DEG C, 950 r/min hybrid reaction 4min, with extruder in 179 DEG C of extruding pelletizations of temperature, that is, obtain polyvinyl chloride carbonized agent.
Embodiment 6
A kind of polyvinyl chloride carbonized agent, its preparation method comprise the following steps：
(1) 5 parts of silica gel, 58 parts of tetraethyl orthosilicates, 55 parts of sodium metasilicate, 10 parts of dodecyl sodium sulfates, 77 parts of water and 137, are weighed
Part ethanol is added in hydrothermal reaction kettle, 9h is reacted under the conditions of 176 DEG C of maintenance system temperature, product is through 1000mL water washings 3
Secondary, 1000mL ethanol washs 3 times, 55 DEG C, -0.09MPa vacuum drying 18min, obtains silica gel improved silica aeroge；
(2), weigh 40 parts of ammonium oxalate, 16 parts of urea hydrochlorides, 64 parts of isopropanols and 66 parts of ethanol to be added in reactor, mixing speed
For 110r/min, 0.8h is reacted under the conditions of 97 DEG C of maintenance system temperature, -0.04MPa, product depressurizes through 100 DEG C, -0.05MPa
0.5h is distilled, obtains urea oxalate；
(3) 60 parts of zeolite powders, 13 parts of sodium metasilicate, 17 parts of calcium dihydrogen phosphates, 26 parts of phenolic resin and 8 parts of cupric oxide, are weighed to add
Into ball mill, drum speed 35r/min, 0.5h is reacted under the conditions of 44 DEG C of maintenance system temperature, product is through 200 DEG C of roastings
2h, 300 DEG C of roasting 2h, 400 DEG C of roasting 2h, 500 DEG C of roasting 2h, 600 DEG C of roasting 2h, 700 DEG C of roasting 3h, that is, obtains zeolite molecules
Sieve；
(4) 60 parts of polyvinyl chloride, 51 parts of ammonium silicates, 15 parts of neopelexes, 13 parts of OP10 and 17 part of polyformaldehyde, are weighed
It is added in high-speed mixer, mixing velocity 900r/min, 4min is reacted under the conditions of 173 DEG C of maintenance system temperature, with extrusion
Machine obtains ammonium silicate modified polyvinyl chloride in 175 DEG C of extruding pelletizations of temperature；
(5) 70 parts of ammonium silicate modified polyvinyl chlorides, 23 parts of zeolite molecular sieves, 39 parts of urea oxalates, 37 parts of silica gel, are weighed and are modified dioxy
SiClx aeroge, 24 parts of stannous pyrophosphates, 5 parts of ferric stearates are added in high-speed mixer, with high-speed mixer in temperature 175
DEG C, 950 r/min hybrid reaction 6min, with extruder in 181 DEG C of extruding pelletizations of temperature, that is, obtain polyvinyl chloride carbonized agent.
Embodiment 7
A kind of polyvinyl chloride carbonized agent, its preparation method comprise the following steps：
(1) 5 parts of silica gel, 52 parts of tetraethyl orthosilicates, 48 parts of sodium metasilicate, 9 parts of dodecyl sodium sulfates, 76 parts of water and 131 parts, are weighed
Ethanol is added in hydrothermal reaction kettle, reacts 7h under the conditions of 183 DEG C of maintenance system temperature, product through 1000mL water washings 3 times,
1000mL ethanol washs 3 times, 55 DEG C, -0.09MPa vacuum drying 18min, obtains silica gel improved silica aeroge；
(2), weigh 40 parts of ammonium oxalate, 12 parts of urea hydrochlorides, 67 parts of isopropanols and 69 parts of ethanol to be added in reactor, mixing speed
For 105r/min, 0.8h is reacted under the conditions of 94 DEG C of maintenance system temperature, -0.04MPa, product depressurizes through 100 DEG C, -0.05MPa
0.5h is distilled, obtains urea oxalate；
(3) 60 parts of zeolite powders, 16 parts of sodium metasilicate, 18 parts of calcium dihydrogen phosphates, 22 parts of phenolic resin and 11 parts of cupric oxide, are weighed to add
Into ball mill, drum speed 33r/min, 0.5h is reacted under the conditions of 47 DEG C of maintenance system temperature, product is through 200 DEG C of roastings
2h, 300 DEG C of roasting 2h, 400 DEG C of roasting 2h, 500 DEG C of roasting 2h, 600 DEG C of roasting 2h, 700 DEG C of roasting 3h, that is, obtains zeolite molecules
Sieve；
(4) 60 parts of polyvinyl chloride, 47 parts of ammonium silicates, 15 parts of neopelexes, 8 parts of OP10 and 16 part of polyformaldehyde, are weighed
It is added in high-speed mixer, mixing velocity 900r/min, 5min is reacted under the conditions of 173 DEG C of maintenance system temperature, with extrusion
Machine obtains ammonium silicate modified polyvinyl chloride in 175 DEG C of extruding pelletizations of temperature；
(5) 70 parts of ammonium silicate modified polyvinyl chlorides, 19 parts of zeolite molecular sieves, 42 parts of urea oxalates, 32 parts of silica gel, are weighed and are modified dioxy
SiClx aeroge, 17 parts of stannous pyrophosphates, 6 parts of ferric stearates are added in high-speed mixer, with high-speed mixer in temperature 175
DEG C, 950 r/min hybrid reaction 6min, with extruder in 182 DEG C of extruding pelletizations of temperature, that is, obtain polyvinyl chloride carbonized agent.
Embodiment 8
A kind of polyvinyl chloride carbonized agent, its preparation method comprise the following steps：
(1) 5 parts of silica gel, 60 parts of tetraethyl orthosilicates, 55 parts of sodium metasilicate, 9 parts of dodecyl sodium sulfates, 76 parts of water and 135 parts, are weighed
Ethanol is added in hydrothermal reaction kettle, reacts 8h under the conditions of 177 DEG C of maintenance system temperature, product through 1000mL water washings 3 times,
1000mL ethanol washs 3 times, 55 DEG C, -0.09MPa vacuum drying 18min, obtains silica gel improved silica aeroge；
(2), weigh 40 parts of ammonium oxalate, 17 parts of urea hydrochlorides, 70 parts of isopropanols and 69 parts of ethanol to be added in reactor, mixing speed
For 108r/min, 0.6h is reacted under the conditions of 98 DEG C of maintenance system temperature, -0.04MPa, product depressurizes through 100 DEG C, -0.05MPa
0.5h is distilled, obtains urea oxalate；
(3) 60 parts of zeolite powders, 13 parts of sodium metasilicate, 17 parts of calcium dihydrogen phosphates, 21 parts of phenolic resin and 12 parts of cupric oxide, are weighed to add
Into ball mill, drum speed 35r/min, 0.5h is reacted under the conditions of 44 DEG C of maintenance system temperature, product is through 200 DEG C of roastings
2h, 300 DEG C of roasting 2h, 400 DEG C of roasting 2h, 500 DEG C of roasting 2h, 600 DEG C of roasting 2h, 700 DEG C of roasting 3h, that is, obtains zeolite molecules
Sieve；
(4) 60 parts of polyvinyl chloride, 50 parts of ammonium silicates, 15 parts of neopelexes, 9 parts of OP10 and 16 part of polyformaldehyde, are weighed
It is added in high-speed mixer, mixing velocity 900r/min, 4min is reacted under the conditions of 173 DEG C of maintenance system temperature, with extrusion
Machine obtains ammonium silicate modified polyvinyl chloride in 175 DEG C of extruding pelletizations of temperature；
(5) 70 parts of ammonium silicate modified polyvinyl chlorides, 31 parts of zeolite molecular sieves, 44 parts of urea oxalates, 39 parts of silica gel, are weighed and are modified dioxy
SiClx aeroge, 15 parts of stannous pyrophosphates, 6 parts of ferric stearates are added in high-speed mixer, with high-speed mixer in temperature 175
DEG C, 950 r/min hybrid reaction 7min, with extruder in 185 DEG C of extruding pelletizations of temperature, that is, obtain polyvinyl chloride carbonized agent.
Reference examples 1
In this reference examples, silica gel improved silica aeroge is not added, and other components and preparation method are same as Example 1.
Reference examples 2
In this reference examples, urea oxalate is not added, other components and preparation method are same as Example 1.
Reference examples 3
In this reference examples, zeolite molecular sieve is not added, other components and preparation method are same as Example 1.
Reference examples 4
In this reference examples, ammonium silicate modified polyvinyl chloride is not added, and other components and preparation method are same as Example 1.
Reference examples 5
In this reference examples, stannous pyrophosphate is not added, other components and preparation method are same as Example 1.
Reference examples 6
In this reference examples, from the silica gel improved silica gas in general silica aeroge alternate embodiment 1 in formula
Gel, other components and preparation method are same as Example 1.
Reference examples 7
In this reference examples, from the urea oxalate in common urea alternate embodiment 1, other components and preparation method and reality in formula
It is identical to apply example 1.
Reference examples 8
In this reference examples, from the zeolite molecular sieve in common zeolite molecular sieve alternate embodiment 1, other components and system in formula
Preparation Method is same as Example 1.
Reference examples 9
In this reference examples, in formula select common polyvinyl chloride alternate embodiment 1 in ammonium silicate modified polyvinyl chloride, other groups
Divide same as Example 1 with preparation method.
The performance parameter of polyvinyl chloride carbonized agent made from the embodiment 1 of table 1 and reference examples 1~9
| Embodiment 1 | Reference examples 1 | Reference examples 2 | Reference examples 3 | Reference examples 4 | Reference examples 5 | Reference examples 6 | Reference examples 7 | Reference examples 8 | Reference examples 9 | |
| 500 DEG C of charring rate/% | 53.2 | 39.7 | 43.7 | 46.7 | 36.4 | 47.3 | 41.8 | 46.5 | 45.9 | 33.8 |
Described above is the preferred embodiment of the invention, it is noted that for those skilled in the art,
On the premise of the inventive principle is not departed from, some improvements and modifications can also be made, these improvements and modifications are also considered as the hair
Bright protection domain.
Claims (3)
- A kind of 1. preparation method of polyvinyl chloride carbonized agent, it is characterised in that：Including following raw material components：Ammonium silicate is modified polychlorostyrene Ethene, zeolite molecular sieve, urea oxalate, silica gel improved silica aeroge, stannous pyrophosphate, ferric stearate, described silicic acid Ammonium modified polyvinyl chloride, zeolite molecular sieve, urea oxalate, silica gel improved silica aeroge, stannous pyrophosphate, ferric stearate Quality parts ratio is 70：19~32：34~46：29~45：13~25：2~7, wherein, described ammonium silicate modified polyvinyl chloride It is made by the reaction of polyvinyl chloride, ammonium silicate, neopelex, OP10 and polyformaldehyde, described polyvinyl chloride, silicic acid Ammonium, neopelex, the quality parts ratio of OP10 and polyformaldehyde are 60：35~52：9~18：7~14：12~20, institute The zeolite molecular sieve stated is reacted by zeolite powder, sodium metasilicate, calcium dihydrogen phosphate, phenolic resin and cupric oxide to be made, described zeolite Powder, sodium metasilicate, calcium dihydrogen phosphate, the quality parts ratio of phenolic resin and cupric oxide are 60：8~17：10~21：16~27：5~ 12, described urea oxalate is made by ammonium oxalate, urea hydrochloride, isopropanol and ethanol synthesis, described ammonium oxalate, urea hydrochloride, isopropyl The quality parts ratio of alcohol and ethanol is 40：11~21：59~71：58~70, described silica gel improved silica aeroge by Silica gel, tetraethyl orthosilicate, sodium metasilicate, dodecyl sodium sulfate, water and ethanol synthesis are made, described silica gel, tetraethyl orthosilicate, Sodium metasilicate, dodecyl sodium sulfate, the quality parts ratio of water and ethanol are 5：45~63：39~56：7~13：64~80：123 ~140.
- A kind of 2. preparation method of polyvinyl chloride carbonized agent according to claim 1, it is characterised in that：Described polyvinyl chloride Carbonized agent is as made from following preparation method：(1), by silica gel, tetraethyl orthosilicate, sodium metasilicate, dodecyl sodium sulfate, water and Ethanol is 5 according to quality parts ratio：45~63：39~56：7~13：64~80：123~140 are added in hydrothermal reaction kettle, 6~13h is reacted under the conditions of 168~185 DEG C of maintenance system temperature, product is through 1000mL water washings 3 times, 1000mL ethanol washing 3 It is secondary, 55 DEG C, -0.09MPa vacuum drying 18min, obtain silica gel improved silica aeroge；(2), by ammonium oxalate, urea hydrochloride, Isopropanol and ethanol are according to quality parts ratio 40：11~21：59~71：58~70 are added in reactor, mixing speed 97 Under the conditions of~117r/min, 93~100 DEG C of maintenance system temperature, -0.04MPa react 0.5~1h, product through 100 DEG C, - 0.05MPa is evaporated under reduced pressure 0.5h, obtains urea oxalate；(3), by zeolite powder, sodium metasilicate, calcium dihydrogen phosphate, phenolic resin and oxidation Copper is according to quality parts ratio 60：8~17：10~21：16~27：5~12 are added in ball mill, and drum speed is 30~36r/ Min, reacts 0.5h under the conditions of 35~51 DEG C of maintenance system temperature, and product is through 200 DEG C of roasting 2h, 300 DEG C of roasting 2h, 400 DEG C of roastings 2h is burnt, 500 DEG C of roasting 2h, 600 DEG C of roasting 2h, 700 DEG C of roasting 3h, that is, obtains zeolite molecular sieve；(4), by polyvinyl chloride, silicic acid Ammonium, neopelex, OP10 and polyformaldehyde are according to quality parts ratio 60：35~52：9~18：7~14：12~20 add Enter into high-speed mixer, mixing velocity 900r/min, under the conditions of 173 DEG C of maintenance system temperature react 2~7min, with squeeze Go out machine in 175 DEG C of extruding pelletizations of temperature, that is, obtain ammonium silicate modified polyvinyl chloride；(5), by ammonium silicate modified polyvinyl chloride, boiling Stone molecular sieve, urea oxalate, silica gel improved silica aeroge, stannous pyrophosphate, ferric stearate are according to quality parts ratio 70：19 ~32：34~46：29~45：13~25：2~7 are added in high-speed mixer, with high-speed mixer in 175 DEG C of temperature, 950 R/min 3~8min of hybrid reaction, with extruder in 174~185 DEG C of extruding pelletizations of temperature, that is, obtain polyvinyl chloride carbonized agent.
- A kind of 3. preparation method of polyvinyl chloride carbonized agent according to claim 2, it is characterised in that：Described zeolite powder mesh Number is 1250 mesh.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103911871A (en) * | 2014-04-23 | 2014-07-09 | 昆山阿基里斯人造皮有限公司 | Method for manufacturing polyvinyl chloride artificial leather with high carbon-forming rate |
| CN103992352A (en) * | 2014-06-11 | 2014-08-20 | 苏州科技学院相城研究院 | PEPA (polymeric pentaerythrityl phosphate) compound as caged tricyclic flame-retardant charring agent and preparation method of PEPA compound |
| CN106045928A (en) * | 2016-05-30 | 2016-10-26 | 南京林业大学 | Method for preparing triazine ring carbon-forming agent containing polyhydroxyl |
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2017
- 2017-10-12 CN CN201710947384.1A patent/CN107603068A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103911871A (en) * | 2014-04-23 | 2014-07-09 | 昆山阿基里斯人造皮有限公司 | Method for manufacturing polyvinyl chloride artificial leather with high carbon-forming rate |
| CN103992352A (en) * | 2014-06-11 | 2014-08-20 | 苏州科技学院相城研究院 | PEPA (polymeric pentaerythrityl phosphate) compound as caged tricyclic flame-retardant charring agent and preparation method of PEPA compound |
| CN106045928A (en) * | 2016-05-30 | 2016-10-26 | 南京林业大学 | Method for preparing triazine ring carbon-forming agent containing polyhydroxyl |
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