CN105733273A - Method for producing tapping paraffin serving as polyurethane foam crack filler - Google Patents
Method for producing tapping paraffin serving as polyurethane foam crack filler Download PDFInfo
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- CN105733273A CN105733273A CN201610268921.5A CN201610268921A CN105733273A CN 105733273 A CN105733273 A CN 105733273A CN 201610268921 A CN201610268921 A CN 201610268921A CN 105733273 A CN105733273 A CN 105733273A
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- chlorine
- temperature
- paraffin
- polyurethane foam
- perforate
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- 239000012188 paraffin wax Substances 0.000 title claims abstract description 78
- 229920005830 Polyurethane Foam Polymers 0.000 title claims abstract description 60
- 239000011496 polyurethane foam Substances 0.000 title claims abstract description 60
- 239000000945 filler Substances 0.000 title claims abstract description 55
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 27
- 238000010079 rubber tapping Methods 0.000 title abstract 4
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 100
- 239000000460 chlorine Substances 0.000 claims abstract description 100
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 100
- 238000006243 chemical reaction Methods 0.000 claims abstract description 56
- 239000007788 liquid Substances 0.000 claims abstract description 49
- 239000001993 wax Substances 0.000 claims abstract description 49
- 238000000034 method Methods 0.000 claims abstract description 25
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000007789 gas Substances 0.000 claims abstract description 17
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims abstract description 17
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000002253 acid Substances 0.000 claims abstract description 11
- 239000002131 composite material Substances 0.000 claims description 15
- 239000003017 thermal stabilizer Substances 0.000 claims description 15
- 238000001514 detection method Methods 0.000 claims description 6
- 239000006260 foam Substances 0.000 abstract description 15
- 230000000694 effects Effects 0.000 abstract description 5
- 230000008901 benefit Effects 0.000 abstract description 2
- 238000007664 blowing Methods 0.000 abstract description 2
- 239000000470 constituent Substances 0.000 abstract 2
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 150000001875 compounds Chemical class 0.000 abstract 1
- 239000012760 heat stabilizer Substances 0.000 abstract 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 15
- HVLLSGMXQDNUAL-UHFFFAOYSA-N triphenyl phosphite Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)OC1=CC=CC=C1 HVLLSGMXQDNUAL-UHFFFAOYSA-N 0.000 description 14
- 230000000630 rising effect Effects 0.000 description 13
- 206010000269 abscess Diseases 0.000 description 11
- 239000000203 mixture Substances 0.000 description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- UWFRVQVNYNPBEF-UHFFFAOYSA-N 1-(2,4-dimethylphenyl)propan-1-one Chemical compound CCC(=O)C1=CC=C(C)C=C1C UWFRVQVNYNPBEF-UHFFFAOYSA-N 0.000 description 7
- 239000004593 Epoxy Substances 0.000 description 7
- 235000012424 soybean oil Nutrition 0.000 description 7
- 239000003549 soybean oil Substances 0.000 description 7
- 230000001276 controlling effect Effects 0.000 description 6
- 230000035699 permeability Effects 0.000 description 5
- -1 polymethylene Polymers 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 4
- 230000009467 reduction Effects 0.000 description 4
- 239000003381 stabilizer Substances 0.000 description 4
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 3
- CLBRCZAHAHECKY-UHFFFAOYSA-N [Co].[Pt] Chemical compound [Co].[Pt] CLBRCZAHAHECKY-UHFFFAOYSA-N 0.000 description 3
- 239000000498 cooling water Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000002932 luster Substances 0.000 description 3
- 229920002545 silicone oil Polymers 0.000 description 3
- 230000000977 initiatory effect Effects 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229920001821 foam rubber Polymers 0.000 description 1
- 239000012948 isocyanate Substances 0.000 description 1
- 150000002513 isocyanates Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L91/00—Compositions of oils, fats or waxes; Compositions of derivatives thereof
- C08L91/06—Waxes
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G73/00—Recovery or refining of mineral waxes, e.g. montan wax
- C10G73/38—Chemical modification of petroleum
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
Landscapes
- Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Polyurethanes Or Polyureas (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
Abstract
The invention discloses a method for producing tapping paraffin serving as polyurethane foam crack filler.The method comprises the following steps of adding heavy liquid wax into a reaction kettle; introducing chlorine into the reaction kettle, and controlling the reaction temperature; after the heavy liquid wax reacts with the chlorine for a while, detecting the density of chlorinated paraffin, and then blowing off hydrogen chloride gas; after the hydrogen chloride gas is blown off, detecting the acid value, and then adding compound heat stabilizer, so that the tapping paraffin is obtained.The method for producing the tapping paraffin has the advantages that the temperature of the reaction conducted between the heavy liquid wax and chlorine and the introducing amount of chlorine are controlled, so that low-carbon-chain constituents maintain low chlorine content, high-carbon-chain constituents have high chlorine content, chlorine elements are uniformly distributed on the heavy liquid wax, the distribution mode is beneficial to foam hole balance of the polyurethane foam crack filler, in addition, foam holes can emerge to be of a netted structure, and untoward effects such as enlarged foam holes and messy foam cannot be caused.
Description
Technical field
The present invention relates to the manufacture method of plasticizer, be specifically related to a kind of perforate paraffin manufacture method for cranny filler of polyurethane foam.
Background technology
Cranny filler of polyurethane foam is a kind of one-component, moisture-curable, multiduty polyurethane foam filling elaxtic seal.The premium properties such as its cured foam elastomer has bonding, waterproof, resistance to expands with heat and contract with cold, heat insulation, sound insulation, are widely used in being filled with a sealing of building doors and windows side seam, member expansion joint and hole place.But under hot and humid environment, its absolutely dry speed can be accelerated, cause that the rate of closed hole of polyurethane foam increases, breathability reduces, and in room temperature situation, Air Temperature Difference expands with heat and contract with cold and can cause the contraction of cranny filler of polyurethane foam, affect the continuous stability of cranny filler of polyurethane foam.
Generally, people slow down the cranny filler of polyurethane foam absolutely dry speed hot and humid when by adding excessive polymethylene multi-phenenyl isocyanate in cranny filler of polyurethane foam, increase percent opening and the breathability of cranny filler of polyurethane foam；Or in cranny filler of polyurethane foam, add price opening silicone oil costly, but after adding opening silicone oil, add percent opening and the breathability of polyurethane foam filler, but the crushing resistance of polyurethane foam filler can be reduced simultaneously, in addition, due to opening silicone oil costly, the price of product will be made to can not get good control.
Summary of the invention
It is an object of the invention to provide the manufacture method of the perforate paraffin of a kind of perforate performance that can increase cranny filler of polyurethane foam and permeability.
A kind of perforate paraffin manufacture method for cranny filler of polyurethane foam, comprises the following steps,
(1) in reactor, heavy liquid wax is added；
(2) in reactor, pass into chlorine, and control the temperature of reaction；
(3) after heavy liquid wax and chlorine reaction a period of time, the density of detection chlorinated paraffin, then carry out stripping hydrogen chloride gas；Heavy liquid wax generates chlorinated paraffin with chlorine reaction, releases hydrogen chloride gas simultaneously, after the density of detection chlorinated paraffin reaches requirement, with the hydrogen chloride gas in Air blowing reactor, i.e. stripping hydrogen chloride gas；
(4) in step (3) after stripping hydrogen chloride gas, detect acid number, be subsequently adding composite thermal stabilizer, both obtain perforate paraffin.
Further, when described heavy liquid wax and chlorine react, reaction temperature is 50-55 DEG C, and the flow that passes into of chlorine is 28-32m3/h.After passing into chlorine in reactor, chlorine reacts with heavy liquid wax, and the reaction of chlorine and heavy liquid wax belongs to exothermic reaction, carrying out along with reaction, temperature in reactor will raise, and before temperature in a kettle. reaches 50-55 DEG C, passes into the flow-control of chlorine at 28-32cm3/ h, generally, after 1.5-2.5h, the temperature in reactor can reach 50-55 DEG C.
Further, when heavy liquid wax described in step (2) and chlorine react, first the flow that passes at 50-55 DEG C, chlorine is 28-32m3When/h react 1.5-2.5h, then regulate temperature to 55-65 DEG C, the flow that passes into of chlorine is 28-32m35.5-6.5h is reacted when/h.The temperature regulating reactor is that the method leading to supercooled water is adjusted, during because passing into chlorine in reactor, chlorine and heavy liquid wax react, temperature in reactor can raise always, at this moment reaction material is lowered the temperature, keep the temperature in reactor at 55-65 DEG C, and react 5.5-6.5h at this temperature.In whole course of reaction, control temperature and slowly rise, because temperature affect the course of reaction of chlorine and heavy liquid wax, along with the rising heavy liquid wax of temperature to the absorbtivity of chlorine also with rising.
Further, heavy liquid wax described in step (2) and chlorine temperature be 55-65 DEG C, the flow that passes into of chlorine be 28-32m3React after 5.5-6.5h when/h, then regulate temperature to 65-75 DEG C, the flow that passes into of chlorine is 38-42m35.5-6.5h is reacted when/h.Because of along with the rising of temperature, heavy liquid wax to the absorbtivity of chlorine also with rising, so controlling while temperature slowly rises, increasing the flow of chlorine, now also leading to supercooled water to control temperature.
Further, heavy liquid wax described in step (2) and chlorine temperature be 65-75 DEG C, the flow that passes into of chlorine be 38-42m3React after 5.5-6.5h when/h, then regulate temperature to 75-85 DEG C, the flow that passes into of chlorine plays 38-42m35.5-6.5h is reacted when/h.
Further, heavy liquid wax described in step (2) and chlorine temperature be 75-85 DEG C, the flow that passes into of chlorine be 38-42m3React after 5.5-6.5h when/h, then regulate temperature to 85-95 DEG C, the flow that passes into of chlorine plays 38-42m313.5-14.5h is reacted when/h.When perforate paraffin is applied in cranny filler of polyurethane foam, the performance of bubble is had brokenly when chlorinty is low, if and the 52# chlorinated paraffin usually used is because viscosity own also can be directly proportional reduction with regard to the little chlorinty viscosity that reduces again, the 52# chlorinated paraffin of such decrease in viscosity does not support cranny filler of polyurethane foam completely and sends the form of foam, and the bubble that causes collapsing, and select the heavy liquid wax of this Long carbon chain as raw material, by controlling the reaction temperature of heavy liquid wax and chlorine, and control the intake of chlorine, produce the perforate paraffin of this perforate performance that can increase cranny filler of polyurethane foam and permeability.In the production process of perforate paraffin of the present invention, initial reaction temperature is low, so control the composition of low carbon chain by temperature and keep relatively low chlorinty, temperature grows steadily, and makes the composition of reaction later stage high carbon chain containing higher chlorine, and carbochain is more high and chlorine reaction out product viscosity is also more big.So, perforate paraffin is used effect of cranny filler of polyurethane foam and is opened abscess exactly, will not shrink because rate of closed hole is high, deformation after making cranny filler of polyurethane foam dry.In addition make the perforate paraffin produced in this way apply in cranny filler of polyurethane foam, the foam structure that polyurethane foam occurs can be made to present network structure, and do not have abscess and become the untoward reaction such as big, string bubble.
Further, in step (3), when at 50 DEG C when, the density of chlorinated paraffin is 1.205-1.22g/cm3Time, then carry out stripping hydrogen chloride gas.
Further, in step (4) when in step (4) when acid number is less than 0.15mgKOH/g, add composite thermal stabilizer.Composite thermal stabilizer used by the present invention be with Ethylene glycol diglycidyl ether and methyl stannum be main stabilizer, triphenyl phosphite and epoxy soybean oil be help steady heat to determine chlorinated paraffin composite thermal stabilizer prepared by agent.
The invention have the benefit that the manufacture method of perforate paraffin of the present invention, the heavy liquid wax selecting Long carbon chain is primary raw material, by controlling the reaction temperature of heavy liquid wax and chlorine, and the intake of chlorine, the composition making low carbon chain keeps relatively low chlorinty, the composition of high carbon chain contains higher chlorinty, namely heavy liquid wax has the absorption chlorine of control, chlorine element is made to be evenly distributed on heavy liquid wax, the structure that this distribution mode is conducive to the abscess balance of polyurathamc foam gap filler and makes abscess occur is network structure, do not have abscess and become big, the untoward reaction such as string bubble.
In addition, perforate paraffin for cranny filler of polyurethane foam of the present invention is added percent opening and the breathability that can increase cranny filler of polyurethane foam in cranny filler of polyurethane foam, can farthest reduce because temperature difference factor affects product quality problem, simple to operate, and use cost is relatively low.
Detailed description of the invention
Embodiment one
A kind of perforate paraffin manufacture method for cranny filler of polyurethane foam, adds heavy liquid wax in reactor, then passes into chlorine in reactor, controls the flow of chlorine at 28m3/ h, heat is released time because of heavy liquid wax and chlorine reaction, along with reaction carrying out, the temperature in reactor can along with rising, when the temperature in reactor is increased to 50 DEG C, it is increased to the general used time 1.5h of this temperature, then control reactor with cooling water, make the temperature in reactor be slowly raised 55 DEG C, and react 5.5h at this temperature, in time period, the flow of chlorine still controls at 28cm3/h。
When temperature in a kettle. is 55 DEG C when, after reaction 5.5h, increase the flow of chlorine, make the flow of chlorine reach 38m3/ h, makes the temperature in reactor be increased to 65 DEG C, and reacts 5.5h at this temperature, time period, is also the method the leading to supercooled water temperature to control in reactor, along with the rising of temperature, heavy liquid wax to the absorbtivity of chlorine also with rising, so increasing the flow of chlorine within the time period.
When temperature in a kettle. is 65 DEG C when, after reaction 5.5h, regulate the temperature in reactor, make the temperature in reactor be increased to 75 DEG C, and react 5.5h at this temperature, within the time period, the flow of chlorine remains unchanged, and logical supercooled water controls the temperature in reactor.
When temperature is 75 DEG C in a kettle. when, after reaction 5.5h, regulate the temperature to 85 DEG C in reactor, and react 14h at this temperature.
The manufacture method of perforate paraffin of the present invention, point different temperatures time period react because: when perforate paraffin is applied in cranny filler of polyurethane foam, the performance of bubble is had brokenly when chlorinty is low, if and the 52# chlorinated paraffin usually used is because viscosity own also can be directly proportional reduction with regard to the little chlorinty viscosity that reduces again, the 52# chlorinated paraffin of such decrease in viscosity does not support cranny filler of polyurethane foam completely and sends the form of foam, and cause that the foam initiating depresses, and select the heavy liquid wax of this Long carbon chain as raw material, by controlling the reaction temperature of heavy liquid wax and chlorine, and control the intake of chlorine, even if viscosity is also very big when chlorinty is the end of compared with, just can produce the perforate paraffin of this perforate performance that can increase cranny filler of polyurethane foam and permeability.In the production process of perforate paraffin of the present invention, initial reaction temperature is low, so control the composition of low carbon chain by temperature and keep relatively low chlorinty, temperature grows steadily, and makes the composition of reaction later stage high carbon chain containing higher chlorine, and carbochain is more high and chlorine reaction out product viscosity is also more big.So, perforate paraffin is used effect of cranny filler of polyurethane foam and is opened abscess exactly, and will not be expanded with heat and contract with cold by environment because of rate of closed hole height after making cranny filler of polyurethane foam dry affects and shrink, and deforms.In addition make the perforate paraffin produced in this way apply in cranny filler of polyurethane foam, the foam structure that polyurethane foam occurs can be made to present network structure, and do not have abscess and become the bad phenomenon such as big, string bubble.
After heavy liquid wax and chlorine reaction, the density of detection chlorinated paraffin, when at 50 DEG C when, the density of chlorinated paraffin is 1.205g/cm3Time, then carry out stripping hydrogen chloride gas.When the acid number that stripping hydrogen chloride gas makes perforate paraffin is 0.15mgKOH/g, then add composite thermal stabilizer, both obtain perforate paraffin.And as comparing preferred embodiment, the composite thermal stabilizer added in the present invention be with Ethylene glycol diglycidyl ether and methyl stannum be main stabilizer, triphenyl phosphite and epoxy soybean oil be help steady heat to determine chlorinated paraffin composite thermal stabilizer prepared by agent, the mass ratio of Ethylene glycol diglycidyl ether, methyl stannum, triphenyl phosphite and epoxy soybean oil is 72:3:10:15.
The technical specification of the perforate paraffin that the present embodiment produces is: color and luster (platinum-cobalt) 200；Density (50 DEG C) 1.205g/cm3；Chlorinity 44%；Viscosity (50 DEG C) 500mpa.s；Heating loss (130 DEG C, 2h) 0.5%；Acid number 0.15mgKOH/g.
Embodiment two
A kind of perforate paraffin manufacture method for cranny filler of polyurethane foam, adds heavy liquid wax in reactor, then passes into chlorine in reactor, controls the flow of chlorine at 30m3/ h, heat is released time because of heavy liquid wax and chlorine reaction, along with reaction carrying out, the temperature in reactor can along with rising, when the temperature in reactor is increased to 52 DEG C, it is increased to the general used time 2h of this temperature, then control reactor with cooling water, make the temperature in reactor be slowly raised 60 DEG C, and react 6h at this temperature, in time period, the flow of chlorine still controls at 30cm3/h。
When temperature in a kettle. is 60 DEG C when, after reaction 6h, increase the flow of chlorine, make the flow of chlorine reach 40m3/ h, makes the temperature in reactor be increased to 70 DEG C, and reacts 6h at this temperature, time period, is also the method the leading to supercooled water temperature to control in reactor, along with the rising of temperature, heavy liquid wax to the absorbtivity of chlorine also with rising, so increasing the flow of chlorine within the time period.
When temperature in a kettle. is 70 DEG C when, after reaction 6h, regulate the temperature in reactor, make the temperature in reactor be increased to 80 DEG C, and react 6h at this temperature, within the time period, the flow of chlorine remains unchanged, and logical supercooled water controls the temperature in reactor.
When temperature is 80 DEG C in a kettle. when, after reaction 6h, regulate the temperature to 90 DEG C in reactor, and react 13.5h at this temperature.
The manufacture method of perforate paraffin of the present invention, point different temperatures time period react because: when perforate paraffin is applied in cranny filler of polyurethane foam, the performance of bubble is had brokenly when chlorinty is low, if and the 52# chlorinated paraffin usually used is because viscosity own also can be directly proportional reduction with regard to the little chlorinty viscosity that reduces again, the 52# chlorinated paraffin of such decrease in viscosity does not support cranny filler of polyurethane foam completely and sends the form of foam, and cause that the foam initiating depresses, and select the heavy liquid wax of this Long carbon chain as raw material, by controlling the reaction temperature of heavy liquid wax and chlorine, and control the intake of chlorine, even if viscosity is also very big when chlorinty is the end of compared with, just can produce the perforate paraffin of this perforate performance that can increase cranny filler of polyurethane foam and permeability.In the production process of perforate paraffin of the present invention, initial reaction temperature is low, so control the composition of low carbon chain by temperature and keep relatively low chlorinty, temperature grows steadily, and makes the composition of reaction later stage high carbon chain containing higher chlorine, and carbochain is more high and chlorine reaction out product viscosity is also more big.So, perforate paraffin is used effect of cranny filler of polyurethane foam and is opened abscess exactly, and will not be expanded with heat and contract with cold by environment because of rate of closed hole height after making cranny filler of polyurethane foam dry affects and shrink, and deforms.In addition make the perforate paraffin produced in this way apply in cranny filler of polyurethane foam, the foam structure that polyurethane foam occurs can be made to present network structure, and do not have abscess and become the bad phenomenon such as big, string bubble.
After heavy liquid wax and chlorine reaction, the density of detection chlorinated paraffin, when the density of chlorinated paraffin reaches 1.215g/cm3Time, then carry out stripping hydrogen chloride gas.When the acid number that stripping hydrogen chloride gas makes reaction is 0.11mgKOH/g, then add composite thermal stabilizer, both obtain perforate paraffin.And as comparing preferred embodiment, the composite thermal stabilizer added in the present invention be with Ethylene glycol diglycidyl ether and methyl stannum be main stabilizer, triphenyl phosphite and epoxy soybean oil be help steady heat to determine chlorinated paraffin composite thermal stabilizer prepared by agent, the mass ratio of Ethylene glycol diglycidyl ether, methyl stannum, triphenyl phosphite and epoxy soybean oil is 72:3:10:15.
The technical specification of the perforate paraffin that the present embodiment produces is: color and luster (platinum-cobalt) 300；Density (50 DEG C) 1.215g/cm3；Chlorinity 45%；Viscosity (50 DEG C) 580mpa.s；Heating loss (130 DEG C, 2h) 0.3%；Acid number 0.11mgKOH/g.
Embodiment three
A kind of perforate paraffin manufacture method for cranny filler of polyurethane foam, adds heavy liquid wax in reactor, then passes into chlorine in reactor, controls the flow of chlorine at 32m3/ h, heat is released time because of heavy liquid wax and chlorine reaction, along with reaction carrying out, the temperature in reactor can along with rising, when the temperature in reactor is increased to 55 DEG C, it is increased to the general used time 2.5h of this temperature, then control reactor with cooling water, make the temperature in reactor be slowly raised 65 DEG C, and react 6.5h at this temperature, in time period, the flow of chlorine still controls at 32cm3/h。
When temperature in a kettle. is 65 DEG C when, after reaction 6.5h, increase the flow of chlorine, make the flow of chlorine reach 42m3/ h, makes the temperature in reactor be increased to 75 DEG C, and reacts 6.5h at this temperature, time period, is also the method the leading to supercooled water temperature to control in reactor, along with the rising of temperature, heavy liquid wax to the absorbtivity of chlorine also with rising, so increasing the flow of chlorine within the time period.
When temperature in a kettle. is 75 DEG C when, after reaction 6.5h, regulate the temperature in reactor, make the temperature in reactor be increased to 85 DEG C, and react 6.5h at this temperature, within the time period, the flow of chlorine remains unchanged, and logical supercooled water controls the temperature in reactor.
When temperature is 85 DEG C in a kettle. when, after reaction 6.5h, regulate the temperature to 95 DEG C in reactor, and react 14.5h at this temperature.
The manufacture method of perforate paraffin of the present invention, point different temperatures time period react because: when perforate paraffin is applied in cranny filler of polyurethane foam, the performance of bubble is had brokenly when chlorinty is low, if and the perforate paraffin usually used is because viscosity own also can be directly proportional reduction with regard to the little chlorinty viscosity that reduces again, the perforate paraffin of such decrease in viscosity does not support cranny filler of polyurethane foam completely and sends the form of foam, and the bubble that causes collapsing, and select the heavy liquid wax of this Long carbon chain as raw material, by controlling the reaction temperature of heavy liquid wax and chlorine, and control the intake of chlorine, even if viscosity is also very big when chlorinty is the end of compared with, just can produce the perforate paraffin of this perforate performance that can increase cranny filler of polyurethane foam and permeability.In the production process of perforate paraffin of the present invention, initial reaction temperature is low, so control the composition of low carbon chain by temperature and keep relatively low chlorinty, temperature grows steadily, and makes the composition of reaction later stage high carbon chain containing higher chlorine, and carbochain is more high and chlorine reaction out product viscosity is also more big.So, perforate paraffin is used effect of cranny filler of polyurethane foam and is opened abscess exactly, and will not be expanded with heat and contract with cold by environment because of rate of closed hole height after making cranny filler of polyurethane foam dry affects and shrink, and deforms.In addition make the perforate paraffin produced in this way apply in cranny filler of polyurethane foam, the foam structure that polyurethane foam occurs can be made to present network structure, and do not have abscess and become the bad phenomenon such as big, string bubble.
After heavy liquid wax and chlorine reaction, the density of detection chlorinated paraffin, when at 50 DEG C when, the density of chlorinated paraffin reaches 1.22g/cm3Time, then carry out stripping hydrogen chloride gas.When the acid number that stripping hydrogen chloride gas makes reaction is 0.1mgKOH/g, then add composite thermal stabilizer, both obtain perforate paraffin.And as comparing preferred embodiment, the composite thermal stabilizer added in the present invention be with Ethylene glycol diglycidyl ether and methyl stannum be main stabilizer, triphenyl phosphite and epoxy soybean oil be help steady heat to determine chlorinated paraffin composite thermal stabilizer prepared by agent, the mass ratio of Ethylene glycol diglycidyl ether, methyl stannum, triphenyl phosphite and epoxy soybean oil is 72:3:10:15.
The technical specification of the perforate paraffin that the present embodiment produces is: color and luster (platinum-cobalt) 400；Density (50 DEG C) 1.22g/cm3；Chlorinity 46%；Viscosity (50 DEG C) 600mpa.s；Heating loss (130 DEG C, 2h) 0.2%；Acid number 0.1mgKOH/g.
The present invention is not limited to above-mentioned preferred forms; anyone can draw other various forms of products under the enlightenment of the present invention; no matter but in its details, do any change, every have same or like with the application like technical scheme, all fall within protection scope of the present invention.
Claims (8)
1. the perforate paraffin manufacture method for cranny filler of polyurethane foam, it is characterised in that comprise the following steps:
(1) in reactor, heavy liquid wax is added；
(2) in reactor, pass into chlorine, and control the temperature of reaction；
(3) after heavy liquid wax and chlorine reaction a period of time, the density of detection chlorinated paraffin, then carry out stripping hydrogen chloride gas；
(4) in step (3) after stripping hydrogen chloride gas, detect acid number, be subsequently adding composite thermal stabilizer, both obtain perforate paraffin.
2. the perforate paraffin manufacture method for cranny filler of polyurethane foam according to claim 1, it is characterised in that in step (2), when described heavy liquid wax and chlorine react, reaction temperature is 50-55 DEG C, and the flow that passes into of chlorine is 28-32m3/h。
3. the perforate paraffin manufacture method for cranny filler of polyurethane foam according to claim 1, it is characterised in that when heavy liquid wax described in step (2) and chlorine react, first the flow that passes at 50-55 DEG C, chlorine is 28-32m3When/h react 1.5-2.5h, then regulate temperature to 55-65 DEG C, the flow that passes into of chlorine is 28-32m35.5-6.5h is reacted when/h.
4. the perforate paraffin manufacture method for cranny filler of polyurethane foam according to claim 3, it is characterised in that heavy liquid wax described in step (2) and chlorine temperature be 55-65 DEG C, the flow that passes into of chlorine be 28-32m3React after 5.5-6.5h when/h, then regulate temperature to 65-75 DEG C, the flow that passes into of chlorine is 38-42m35.5-6.5h is reacted when/h.
5. the perforate paraffin manufacture method for cranny filler of polyurethane foam according to claim 4, it is characterised in that heavy liquid wax described in step (2) and chlorine temperature be 65-75 DEG C, the flow that passes into of chlorine be 38-42m3React after 5.5-6.5h when/h, then regulate temperature to 75-85 DEG C, the flow that passes into of chlorine plays 38-42m35.5-6.5h is reacted when/h.
6. the perforate paraffin manufacture method for cranny filler of polyurethane foam according to claim 5, it is characterised in that heavy liquid wax described in step (2) and chlorine temperature be 75-85 DEG C, the flow that passes into of chlorine be 38-42m3React after 5.5-6.5h when/h, then regulate temperature to 85-95 DEG C, the flow that passes into of chlorine plays 38-42m313.5-14.5h is reacted when/h.
7. the perforate paraffin manufacture method for cranny filler of polyurethane foam according to claim 6, it is characterised in that in step (3) when at 50 DEG C when, the density of chlorinated paraffin is 1.205-1.22g/cm3Time, then carry out stripping hydrogen chloride gas.
8. the perforate paraffin manufacture method for cranny filler of polyurethane foam according to claim 1, it is characterised in that: in step (4) when acid number is less than 0.15mgKOH/g, add composite thermal stabilizer.
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| CN109022034B (en) * | 2018-05-31 | 2021-02-23 | 石家庄东翔化工有限公司 | Preparation method of flame-retardant paraffin for polyurethane foam gap filler |
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| CN105733273B (en) | 2018-03-02 |
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Denomination of invention: Preparation method of open cell paraffin used for polyurethane foam sealant Granted publication date: 20180302 Pledgee: China Postal Savings Bank Co.,Ltd. Shenze County Branch Pledgor: SHIJIAZHUANG DONGXIANG CHEMICAL Co.,Ltd. Registration number: Y2024980035368 |
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