CN104449328A - Production technology for low-VOC polyurethane home decoration paint - Google Patents
Production technology for low-VOC polyurethane home decoration paint Download PDFInfo
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- CN104449328A CN104449328A CN201310432984.6A CN201310432984A CN104449328A CN 104449328 A CN104449328 A CN 104449328A CN 201310432984 A CN201310432984 A CN 201310432984A CN 104449328 A CN104449328 A CN 104449328A
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- tolylene diisocyanate
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
- C09D175/14—Polyurethanes having carbon-to-carbon unsaturated bonds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
- C08G18/3203—Polyhydroxy compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/34—Carboxylic acids; Esters thereof with monohydroxyl compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/36—Hydroxylated esters of higher fatty acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/76—Polyisocyanates or polyisothiocyanates cyclic aromatic
- C08G18/7614—Polyisocyanates or polyisothiocyanates cyclic aromatic containing only one aromatic ring
- C08G18/7621—Polyisocyanates or polyisothiocyanates cyclic aromatic containing only one aromatic ring being toluene diisocyanate including isomer mixtures
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Polyurethanes Or Polyureas (AREA)
Abstract
A disclosed production technology for low-VOC polyurethane home decoration paint comprises the following steps: (1) successively adding toluene diisocyanate and trimethylol propane with the molar ratio of 4:1 into a reaction kettle, then adding butyle acetate with the concentration of 20%, controlling the temperature to be 60 DEG C if the temperature starts to rise, reacting for 6 h, adding an organic tin solution as a dryer during reaction, stirring, keeping the temperature of 60 DEG C for 3 h, so as to obtain a paint composition A; (2) performing extraction separation; (3) performing recycling utilization; (4) preparing a paint composition B; (5) metering and mixing the paint composition A and the composition B; and (6) diluting. The production technology is reasonable in technology. By selecting trimethylol propane, butyle acetate and other substances with relatively small toxicity as raw materials, generation and volatilization of harmful substances are generated by controlling the raw material ratio, the reaction temperature and the reaction time. By taking the organic tin solution as the dryer, the defects such as gelatination, crusting and the like possibly generated in storage and transportation processes are effectively solved, and product quality is guaranteed.
Description
Technical field
The production technique of the family's coatings that the present invention relates to, particularly relates to the production technique of a kind of low VOC urethane man coatings.
Background technology
VOC is the abbreviation of volatile organic compounds, polyurethane coating, i.e. carbamate coating, belong to VOC category, it is coated with in membrane molecule containing a considerable amount of polyurethane ester bond, it is a kind of excellent property, widely used coating, the main raw material(s) isocyanic ester producing polyurethane coating belongs to noxious chemical, volatile, be detrimental to health, respiratory system is stimulated after suction, cause dry cough, laryngalgia, the micro-vulcabond of long-term suction will cause headache, bronchitis and asthma, serious meeting causes death, simultaneously, the toluene used in polyurethane coating curing agent, the organic solvents such as dimethylbenzene are very large to the murder by poisoning of human body, it can destroy the function of human body hemopoietic system, other solvent also has toxicity in various degree, the health of harm humans, urgent need finds low VOC, the alternative materials of nontoxic or micro-poison and production technique, application number is that CN201010141800.7 discloses a kind of polyurethane coating production technique, the invention provides polyurethane coating, comprise the polyurethane(s) of 80% ~ 90%, the height connection agent of 3% ~ 6%, the fire retardant of 1% ~ 2%, the catalyzer of 2% ~ 6%, the whipping agent of 1% ~ 3%, the suds-stabilizing agent of 2% ~ 4%, described polyurethane(s) is that polyether resin containing alkyl and isocyanic ester radical reaction generate, described whipping agent is that isocyanate and water react the carbonic acid gas generated, this process components is simple, cost compare is low, manufacture craft is simple, and good product quality, but this coating easily produces hazard VOCs, isocyanate group can evaporate in reaction process, not environmentally, the use of high agent easily causes coating to harden in addition, be difficult to recycling.
Summary of the invention
For overcoming the deficiency in prior art, the object of the invention is to provide the production technique of a kind of low VOC urethane man coatings.
For realizing object of the present invention, technical scheme of the present invention is as follows:
A production technique for low VOC urethane man coatings, comprises the steps:
(1) in reactor, tolylene diisocyanate, TriMethylolPropane(TMP) is added successively, tolylene diisocyanate and TriMethylolPropane(TMP) mol ratio are 4:1, add the N-BUTYL ACETATE of 20% again, temperature of reaction is 60 DEG C, reaction times is 6h, adds organotin solution as siccative, and stir in reaction process, at 60 DEG C, be incubated 3h, obtain coating composition first;
(2) extracting and separating, selects the mixed solution of 120# gasoline and benzene as extraction liquid, the tolylene diisocyanate of the unbound state in continuous extraction separating step (1) component first;
(3) recycle, extraction mixed solution decompression step (2) obtained is extracted out or is pressed in distil container with pressurized air, steam extraction liquid by distillation method, residual after distillation be the mixing liquid of unreacted tolylene diisocyanate and a small amount of extraction liquid, recovery tolylene diisocyanate;
(4) in reactor, drop into 20% tetramethylolmethane, 30%C5-C9 low carbon acid, 18% phthalic anhydride, 10% refined caster oil, 12% phenylformic acid, stir, before reaction, pass into CO
2gas, surplus air in emptying reactor, after material all dissolves, stirs and passes into water coolant, being warmed up to 200
oc-230
oc, under this condition esterification 3h, when product acid number is less than 10KOHmg/g, as reaction end, be cooled to 130
oc, cools to obtain component second;
(5) measure blended, first, the second component of step (1) and step (4) gained is mixed to get the third component according to the metered proportions of 4:5, in mixing process, adds the 201# silicone oil being dissolved in 25% solution and 0.1% be mixed with in pimelinketone by Nitrocellulose;
(6) dilute, in the third component that step (5) obtains, the mixed solvent adding pimelinketone, N-BUTYL ACETATE and hexanaphthene, as weighting agent, obtains low VOC urethane man coatings;
Preferably, in described step (1), described organotin solution is the dibutyl tin laurate solution of 0.01%-0.03%.
Preferably, in described step (2), the metering ratio of described 120# gasoline and benzene is 7.5-8.5:2.
Preferably, in described step (6), the metering ratio of described thinner cyclohexanone, N-BUTYL ACETATE and hexanaphthene is 5-5.5:1:4.
Beneficial effect: the present invention is prepared by first component, extracting and separating, recycle, prepared by second component, metering mixing, dilution, packaging seven large steps complete the production technique of low VOC urethane man coatings, select TriMethylolPropane(TMP), the material that the toxicity such as N-BUTYL ACETATE are less makes raw material, by controlling proportioning raw materials, temperature of reaction, soaking time, reduce generation and the volatilization of objectionable impurities, in addition tolylene diisocyanate and TriMethylolPropane(TMP) adduct nontoxic, under the effect of siccative, better carry out addition reaction, level of response is large, pollute few, organotin solution is as siccative, effectively solve the gel that coating may occur in storage and transportation, the defects such as skinning, ensure that the quality of product, sequential extractions is adopted in extraction separation process, and selected the mixed solution of 120# gasoline and benzene as extraction liquid, can well by the extraction of free toluene diisocyanate monomer, the content of tolylene diisocyanate in coating has been reduced to 0.6%-0.66%, reduce the pollution to environment, adopt pimelinketone, N-BUTYL ACETATE and cyclohexane give are thinner, replace the toluene in original technology and dimethylbenzene, the VOC of urethane man coatings has been dropped to bottom line, reach environmental requirement, the second component that raw material prepares coating is done with C5-C9 low carbon acid, not only good than the performance of the second component using oils in building-up process, and production cost is relatively low.
Embodiment
The technique means realized for making the present invention, creation characteristic, reach object and effect is easy to understand, below
In conjunction with embodiment, set forth the present invention further.
Embodiment 1:
The production technique of a kind of low VOC urethane man coatings of the present embodiment, comprises the steps:
(1) in reactor, tolylene diisocyanate, TriMethylolPropane(TMP) is added successively, tolylene diisocyanate and TriMethylolPropane(TMP) mol ratio are 4:1, add the N-BUTYL ACETATE of 20% again, temperature of reaction is 60 DEG C, reaction times is 6h, adds organotin solution as siccative, and stir in reaction process, at 60 DEG C, be incubated 3h, obtain coating composition first;
(2) extracting and separating, selects the mixed solution of 120# gasoline and benzene as extraction liquid, the tolylene diisocyanate of the unbound state in continuous extraction separating step (1) component first;
(3) recycle, extraction mixed solution decompression step (2) obtained is extracted out or is pressed in distil container with pressurized air, steam extraction liquid by distillation method, residual after distillation be the mixing liquid of unreacted tolylene diisocyanate and a small amount of extraction liquid, recovery tolylene diisocyanate;
(4) in reactor, drop into 20% tetramethylolmethane, 30%C5-C9 low carbon acid, 18% phthalic anhydride, 10% refined caster oil, 12% phenylformic acid, stir, before reaction, pass into CO
2gas, surplus air in emptying reactor, after material all dissolves, stirs and passes into water coolant, being warmed up to 200
oc-230
oc, under this condition esterification 3h, when product acid number is less than 10KOHmg/g, as reaction end, be cooled to 130
oc, cools to obtain component second;
(5) measure blended, first, the second component of step (1) and step (4) gained is mixed to get the third component according to the metered proportions of 4:5, in mixing process, adds the 201# silicone oil being dissolved in 25% solution and 0.1% be mixed with in pimelinketone by Nitrocellulose;
(6) dilute, in the third component that step (5) obtains, the mixed solvent adding pimelinketone, N-BUTYL ACETATE and hexanaphthene, as weighting agent, obtains low VOC urethane man coatings;
Wherein, in described step (1), described organotin solution is the dibutyl tin laurate solution of 0.01%, crucially, in described step (2), the metering ratio of described 120# gasoline and benzene is 7.5:2, and, in described step (6), the metering of described thinner cyclohexanone, N-BUTYL ACETATE and hexanaphthene is than being 5:1:4.
Embodiment 2: all the other are identical with described embodiment 1, difference is, in step (1), described organotin solution is the dibutyl tin laurate solution of 0.03%, in described step (2), the metering of described 120# gasoline and benzene is than being 8.5:2, and in described step (6), the metering of described thinner cyclohexanone, N-BUTYL ACETATE and hexanaphthene is than being 5.5:1:4.
Embodiment 3: all the other are identical with described embodiment 1, difference is, in step (1), described organotin solution is the dibutyl tin laurate solution of 0.02%, in described step (2), the metering of described 120# gasoline and benzene is than being 8:2, and in described step (6), the metering of described thinner cyclohexanone, N-BUTYL ACETATE and hexanaphthene is than being 5:1:4.
In above-mentioned three embodiments, in coating, the content of tolylene diisocyanate has been reduced to 0.6%-0.66%, and tolylene diisocyanate is easy to extracting and separating, and the phenomenon such as gel, precipitation, skinning of coating obviously reduces, coating physico-chemical property is excellent, glossy, in temperature 50
oc-60
ostronger thermotolerance is still had within the scope of C.
Comparative example 1: all the other are identical with described embodiment 1, difference is, changes tolylene diisocyanate and TriMethylolPropane(TMP) mol ratio into 3:1 in step (1), and the first component viscosity of generation is large, be difficult to extracting and washing, the tolylene diisocyanate of separated free is more difficult; And synthesizing the first component molecular amount reduction obtained, viscosity reduces, and the tolylene diisocyanate of separated free is more difficult.
Known in practical application, prepared by first component, extracting and separating, recycle, prepared by second component, metering mixing, dilution, packaging seven large steps complete the production technique of low VOC urethane man coatings, select TriMethylolPropane(TMP), the material that the toxicity such as N-BUTYL ACETATE are less makes raw material, by controlling proportioning raw materials, temperature of reaction, soaking time, reduce generation and the volatilization of objectionable impurities, organotin solution is as siccative, effectively solve the gel that coating may occur in storage and transportation, the defects such as skinning, ensure that the quality of product, sequential extractions is adopted in extraction separation process, and selected the mixed solution of 120# gasoline and benzene as extraction liquid, can well by the extraction of free toluene diisocyanate monomer, the content of tolylene diisocyanate in coating has been reduced to 0.6%-0.66%, reduce the pollution to environment, adopt pimelinketone, N-BUTYL ACETATE and cyclohexane give are thinner, replace the toluene in original technology and dimethylbenzene, the VOC of urethane man coatings has been dropped to bottom line, reach environmental requirement, the second component that raw material prepares coating is done with C5-C9 low carbon acid, not only good than the performance of the second component using oils in building-up process, and production cost is relatively low.
The foregoing is only embodiments of the invention; not thereby the scope of the claims of the present invention is limited; every utilize specification sheets of the present invention to do equivalent structure or the conversion of equivalent flow process, or be directly or indirectly used in other relevant technical fields, be all in like manner included in scope of patent protection of the present invention.
Claims (4)
1. a production technique for low VOC urethane man coatings, is characterized in that, comprise the steps:
(1) in reactor, tolylene diisocyanate, TriMethylolPropane(TMP) is added successively, tolylene diisocyanate and TriMethylolPropane(TMP) mol ratio are 4:1, add the N-BUTYL ACETATE of 20% again, temperature of reaction is 60 DEG C, reaction times is 6h, adds organotin solution as siccative, and stir in reaction process, at 60 DEG C, be incubated 3h, obtain coating composition first;
(2) extracting and separating, selects the mixed solution of 120# gasoline and benzene as extraction liquid, the tolylene diisocyanate of the unbound state in continuous extraction separating step (1) component first;
(3) recycle, extraction mixed solution decompression step (2) obtained is extracted out or is pressed in distil container with pressurized air, steam extraction liquid by distillation method, residual after distillation be the mixing liquid of unreacted tolylene diisocyanate and a small amount of extraction liquid, recovery tolylene diisocyanate;
(4) in reactor, drop into 20% tetramethylolmethane, 30%C5-C9 low carbon acid, 18% phthalic anhydride, 10% refined caster oil, 12% phenylformic acid, stir, before reaction, pass into CO
2gas, surplus air in emptying reactor, after material all dissolves, stirs and passes into water coolant, being warmed up to 200
oc-230
oc, under this condition esterification 3h, when product acid number is less than 10KOHmg/g, as reaction end, be cooled to 130
oc, cools to obtain coating composition second;
(5) measure blended, first, the second component of step (1) and step (4) gained is mixed to get the third component according to the metered proportions of 4:5, in mixing process, adds the 201# silicone oil being dissolved in 25% solution and 0.1% be mixed with in pimelinketone by Nitrocellulose;
(6) dilute, in the third component that step (5) obtains, the mixed solvent adding pimelinketone, N-BUTYL ACETATE and hexanaphthene, as weighting agent, obtains coating.
2. the production technique of low VOC urethane man according to claim 1 coatings, is characterized in that, in described step (1), described organotin solution is the dibutyl tin laurate solution of 0.01%-0.03%.
3. the production technique of low VOC urethane man according to claim 1 coatings, is characterized in that, in described step (2), the metering ratio of described 120# gasoline and benzene is 7.5-8.5:2.
4. the production technique of low VOC urethane man according to claim 1 coatings, is characterized in that, in described step (6), the metering ratio of described thinner cyclohexanone, N-BUTYL ACETATE and hexanaphthene is 5-5.5:1:4.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310432984.6A CN104449328A (en) | 2013-09-23 | 2013-09-23 | Production technology for low-VOC polyurethane home decoration paint |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310432984.6A CN104449328A (en) | 2013-09-23 | 2013-09-23 | Production technology for low-VOC polyurethane home decoration paint |
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| Publication Number | Publication Date |
|---|---|
| CN104449328A true CN104449328A (en) | 2015-03-25 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310432984.6A Pending CN104449328A (en) | 2013-09-23 | 2013-09-23 | Production technology for low-VOC polyurethane home decoration paint |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113214697A (en) * | 2021-06-18 | 2021-08-06 | 中国船舶重工集团公司第七二五研究所 | Organic silicon foaming connection coating and preparation method thereof |
| CN114195974A (en) * | 2021-12-06 | 2022-03-18 | 季华实验室 | Polyurethane prepolymer and preparation method thereof, and polyurethane product |
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| GB947973A (en) * | 1961-03-28 | 1964-01-29 | Beck & Company G M B H Dr | Improvements in or relating to polyurethane lacquers |
| US5912299A (en) * | 1995-06-07 | 1999-06-15 | The Sherwin-Williams Company | Coating compositions from oil modified polyurethane dispersions |
| CN1425727A (en) * | 2003-01-08 | 2003-06-25 | 中国科学院水生生物研究所 | Environment protection polyurethane terrace self levelling paint varnish and preparing method |
| CN102643416A (en) * | 2012-05-08 | 2012-08-22 | 合众（佛山）化工有限公司 | Isocyanate modified alkyd resin and preparation method thereof |
| CN103113553A (en) * | 2013-01-30 | 2013-05-22 | 上海市医药保健品进出口有限公司 | Pure vegetable oil based polyalcohol and preparation method thereof |
-
2013
- 2013-09-23 CN CN201310432984.6A patent/CN104449328A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB947973A (en) * | 1961-03-28 | 1964-01-29 | Beck & Company G M B H Dr | Improvements in or relating to polyurethane lacquers |
| US5912299A (en) * | 1995-06-07 | 1999-06-15 | The Sherwin-Williams Company | Coating compositions from oil modified polyurethane dispersions |
| CN1425727A (en) * | 2003-01-08 | 2003-06-25 | 中国科学院水生生物研究所 | Environment protection polyurethane terrace self levelling paint varnish and preparing method |
| CN102643416A (en) * | 2012-05-08 | 2012-08-22 | 合众（佛山）化工有限公司 | Isocyanate modified alkyd resin and preparation method thereof |
| CN103113553A (en) * | 2013-01-30 | 2013-05-22 | 上海市医药保健品进出口有限公司 | Pure vegetable oil based polyalcohol and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 孙德彬: "环保家装涂料——低VOC聚氨酯生产及施工工艺的研究", 《中国优秀博硕士学位论文全文数据库（硕士） 工程科技Ⅰ辑》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113214697A (en) * | 2021-06-18 | 2021-08-06 | 中国船舶重工集团公司第七二五研究所 | Organic silicon foaming connection coating and preparation method thereof |
| CN114195974A (en) * | 2021-12-06 | 2022-03-18 | 季华实验室 | Polyurethane prepolymer and preparation method thereof, and polyurethane product |
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Application publication date: 20150325 |