CN105153987A - Process for producing glue by adopting phthalic anhydride series polyatomic alcohol as raw material - Google Patents
Process for producing glue by adopting phthalic anhydride series polyatomic alcohol as raw material Download PDFInfo
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- CN105153987A CN105153987A CN201510646049.9A CN201510646049A CN105153987A CN 105153987 A CN105153987 A CN 105153987A CN 201510646049 A CN201510646049 A CN 201510646049A CN 105153987 A CN105153987 A CN 105153987A
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- phthalic anhydride
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Abstract
The invention discloses a process for producing glue by adopting phthalic anhydride series polyatomic alcohol as a raw material, and belongs to the technical field of glue production processes. The process comprises the following steps: dehydrating phthalic anhydride series polyatomic alcohol and adipic acid series polyatomic alcohol or phthalic anhydride series polyatomic alcohol and phthalic anhydride oxalic acid for 1-3 hours at 100-120 DEG C to obtain a mixture I; cooling the mixture I, mixing the cooled mixture I with one or more small molecular chain extenders as well as part of aromatic polyisocyanate, an environment-friendly solvent and a catalyst to obtain a mixture II, and putting the mixture II in a reactor; injecting nitrogen gas into the reactor, heating to 75-85 DEG C with a heating device, and carrying out 2 hours' stirring with a stirrer; dropwise adding aromatic polyisocyanate, the environment-friendly solvent and the catalyst continuously, injecting nitrogen gas again, heating to 75-85 DEG C again with the heating device, and carrying out several hours' stirring with the stirrer. The process has the advantages that phthalic anhydride series polyatomic alcohol is adopted as the raw material, and the chain extenders and polyisocyanate are also adopted; the glue, namely a high-component and relatively-high-rigidity polyester-type polyurethane adhesive, is prepared by adding polyisocyanate in a distributed manner in the presence of the environment-friendly solvent, the catalyst and other solvents.
Description
Technical field
The invention belongs to glue Manufacturing Techniques field, be specifically related to a kind ofly be raw material with phthalic anhydride system polyvalent alcohol glue manufacture craft is relevant.
Background technology
Object bonding, realizes by the pulling force between the polymer body in glue.The existing manufacture craft time is longer, requires comparatively large to material usage, also has waste to a certain degree, also have a certain impact simultaneously to environment aspect to the consumption of the energy.For this problem, applicant research and develop a kind of with phthalic anhydride polyol be raw material caking ability high, there is water tolerance and non yellowing and be applicable to the glue manufacture craft in the higher gluing field of hardness.
Summary of the invention
Object of the present invention be intended to overcome provide a kind of with phthalic anhydride system polyvalent alcohol for raw material caking ability is high, there is water tolerance and non yellowing and be applicable to the glue manufacture craft in the higher gluing field of hardness.
For this reason, the present invention by the following technical solutions: a kind of glue manufacture craft that is raw material with phthalic anhydride system polyvalent alcohol, it is characterized in that, described glue manufacture craft comprises the following steps:
1, dewater phthalic anhydride system polyvalent alcohol and adipic acid system polyvalent alcohol or phthalic anhydride system polyvalent alcohol and phthalic anhydride oxalic acid under 100-120 degree Celsius 1-3 hour, after cooling and small molecule chain extender and partially aromatic polyisocyanates, environment-friendly type solvent and catalyst mix put into reactor, nitrogen will be passed into and by between heating devices heat to 75-85 degree in reactor, and stirred by agitator, continue two hours;
2, continue to drip as above-mentioned consistent aromatic polyisocyanate, environment-friendly type solvent and catalyzer, pass into nitrogen and by between heating devices heat to 75-85 degree, and stirred by agitator, continue two hours;
3, continue to drip as above-mentioned consistent aromatic polyisocyanate, environment-friendly type solvent and catalyzer, pass into nitrogen and by between heating devices heat to 75-85 degree, and stirred by agitator, continue two hours;
4, finally drip once environment-friendly type solvent described above and catalyzer again, then add antioxidant, ultraviolet absorbers, pass into nitrogen and by between heating devices heat to 75-85 degree, and stirred by agitator, continue two hours;
5, by the also discharging of the greenhouse cooling to 70 of reactor degree after having reacted.
Use the present invention can reach following beneficial effect: the present invention is raw material and chainextender and polyisocyanates by phthalic anhydride system polyvalent alcohol, under the condition of environment-friendly type solvent, catalysts and solvents, polyisocyanates is added by distribution, prepare high component and the higher Polyester polyurethane adhesive of hardness, can be used for an electric car, petrochemical complex, material of construction, furniture industry, can be used for refrigerator insulation, sterilizing-cabinet, freezer, refrigerator car, piping insulation cold insulation, building board, imitative wooden furniture, tackiness agent, soles system, the field such as plastic cement race track and spray material.
Embodiment
Embodiment 1:1, dewater phthalic anhydride system polyvalent alcohol and adipic acid system polyvalent alcohol under 100-120 degree Celsius 1-3 hour, after cooling and small molecule chain extender and partially aromatic polyisocyanates, environment-friendly type solvent and catalyst mix put into reactor, nitrogen will be passed into and by between heating devices heat to 75-85 degree in reactor, and stirred by agitator, continue two hours;
2, continue to drip as above-mentioned consistent aromatic polyisocyanate, environment-friendly type solvent and catalyzer, pass into nitrogen and by between heating devices heat to 75-85 degree, and stirred by agitator, continue two hours;
3, continue to drip as above-mentioned consistent aromatic polyisocyanate, environment-friendly type solvent and catalyzer, pass into nitrogen and by between heating devices heat to 75-85 degree, and stirred by agitator, continue two hours;
4, finally drip once environment-friendly type solvent described above and catalyzer again, then add antioxidant, ultraviolet absorbers, pass into nitrogen and by between heating devices heat to 75-85 degree, and stirred by agitator, continue two hours;
5, by the also discharging of the greenhouse cooling to 70 of reactor degree after having reacted.
Embodiment 2,1, dewater phthalic anhydride system polyvalent alcohol and phthalic anhydride oxalic acid under 100-120 degree Celsius 1-3 hour, after cooling and small molecule chain extender and partially aromatic polyisocyanates, environment-friendly type solvent and catalyst mix put into reactor, nitrogen will be passed into and by between heating devices heat to 75-85 degree in reactor, and stirred by agitator, continue two hours;
2, continue to drip as above-mentioned consistent aromatic polyisocyanate, environment-friendly type solvent and catalyzer, pass into nitrogen and by between heating devices heat to 75-85 degree, and stirred by agitator, continue two hours;
3, continue to drip as above-mentioned consistent aromatic polyisocyanate, environment-friendly type solvent and catalyzer, pass into nitrogen and by between heating devices heat to 75-85 degree, and stirred by agitator, continue two hours;
4, finally drip once environment-friendly type solvent described above and catalyzer again, then add antioxidant, ultraviolet absorbers, pass into nitrogen and by between heating devices heat to 75-85 degree, and stirred by agitator, continue two hours;
5, by the also discharging of the greenhouse cooling to 70 of reactor degree after having reacted.
As to above-mentioned steps preferably, aromatic polyisocyanate, environment-friendly type solvent and catalyzer are dripped by even Dropping feeder.Above-mentioned small molecule chain extender accounts for the 0.1-1 ‰ of total mass ratio, is preferably 0.5 ‰.The dripping quantity of above-mentioned aromatic polyisocyanate is the-NCO in isocyanic ester is 0.9-1.0 with the alcoholic extract hydroxyl group mol ratio of above-mentioned raw materials;-NCO in aromatic polyisocyanate is 0.995 with the hydroxyl preferred molar ratio of above-mentioned raw materials.
Preferably, environment-friendly type solvent is one or both and the above combination in methylcarbonate, propylene carbonate, ethylene dimethyl, Methyl glutarate, succinic acid diformazan.
At least one in the group that above-mentioned aromatic polyisocyanate forms primarily of tolylene diisocyanate (TDI), '-diphenylmethane diisocyanate (MDI), tetramethylxylene two isocyanic acid acid esters (TMXDAI) and many phenyl many subunits vulcabond (PAPI); Except aromatic polyisocyanate, also can adopt aliphatic polyisocyanates, aliphatic polyisocyanates weather resisteant is excellent, mainly contains hexamethylene diisocyanate (HDI), isophorone diisocyanate (IPDI), two ring ethyl methane vulcabond (HMDI) etc.
Catalyzer mainly comprises tertiary amines and metallic compound, although-NCO is high with alcoholic extract hydroxyl group-OH reactive behavior in vulcabond, easily carry out, but in order to Reaction time shorten, reaction is guided to carry out along the direction along expection, need in reaction to add a small amount of catalyzer, conventional catalyzer has tertiary amines, metallic compound and organophosphorus.The catalytic activity of different catalysts is different, and tertiary amine has remarkable katalysis to aromatic series TDI, but extremely weak to aliphatic HDI katalysis; Metallic compound has strong katalysis to aromatic series and aliphatic isocyanic ester, but zinc naphthenate is weak to aromatic series TDI katalysis, stronger to aliphatic HDI effect.In fact, custom catalysts is dibutyl tin laurate and stannous octoate, and its consumption is 0.01% ~ 1% of total charging capacity.
Further, antioxidant is 2,6-di-t-butyl one cresylol (antioxidant 264), four (4-hydroxyl-3,5-tert-butyl-phenyl propionic acid) pentaerythritol ester (antioxidant 1010), 3.5-di-t-butyl-4-hydroxy phenylpropionic acid octadecyl ester (antioxidant 1076), triphenyl phosphite (TPP), tricresyl phosphite (nonyl benzene) ester (TNP).Ultraviolet absorbers is UV-24 or UV-9 or Salol or OPS or BAD or UV-P or UV-236.Above-mentioned interpolation antioxidant and UV light absorber, can improve the performance of the anti-oxidant of glue and ultraviolet radiation preventing.
More than show and describe ultimate principle of the present invention and principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and specification sheets just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.Application claims protection domain is defined by appending claims and equivalent thereof.
Claims (9)
1. with the glue manufacture craft that phthalic anhydride system polyvalent alcohol is raw material, it is characterized in that: described glue manufacture craft comprises the following steps:
1), dewater phthalic anhydride system polyvalent alcohol and adipic acid system polyvalent alcohol or phthalic anhydride system polyvalent alcohol and phthalic anhydride oxalic acid under 100-120 degree Celsius 1-3 hour, after cooling and small molecule chain extender and partially aromatic polyisocyanates, environment-friendly type solvent and catalyst mix put into reactor, nitrogen will be passed into and by between heating devices heat to 75-85 degree in reactor, and stirred by agitator, continue two hours;
2), continue to drip as above-mentioned consistent aromatic polyisocyanate, environment-friendly type solvent and catalyzer, pass into nitrogen and by between heating devices heat to 75-85 degree, and stirred by agitator, continue two hours;
3), continue to drip as above-mentioned consistent aromatic polyisocyanate, environment-friendly type solvent and catalyzer, pass into nitrogen and by between heating devices heat to 75-85 degree, and stirred by agitator, continue two hours;
4), finally drip once environment-friendly type solvent described above and catalyzer again, then add antioxidant, ultraviolet absorbers, pass into nitrogen and by between heating devices heat to 75-85 degree, and stirred by agitator, continue two hours;
5) by the also discharging of the greenhouse cooling to 70 of reactor degree after, having reacted.
2. a kind of glue manufacture craft that is raw material with phthalic anhydride system polyvalent alcohol according to claim 1, is characterized in that: described aromatic polyisocyanate, environment-friendly type solvent and catalyzer are dripped by even Dropping feeder.
3. a kind of glue manufacture craft that is raw material with phthalic anhydride system polyvalent alcohol according to claim 1, is characterized in that: the dripping quantity of described aromatic polyisocyanate is the-NCO in isocyanic ester is 0.9-1.0 with the alcoholic extract hydroxyl group mol ratio of above-mentioned raw materials.
4. a kind of glue manufacture craft that is raw material with phthalic anhydride system polyvalent alcohol according to claim 3, is characterized in that: the dripping quantity of described aromatic polyisocyanate is the-NCO in isocyanic ester is 0.995 with the alcoholic extract hydroxyl group mol ratio of above-mentioned raw materials.
5. a kind of glue manufacture craft that is raw material with phthalic anhydride system polyvalent alcohol according to claim 1, it is characterized in that: described small molecule chain extender is ethylene glycol, 1, 2-propylene glycol, 1, 3-propylene glycol, 1, 4-butyleneglycol, 2-methyl-1, 3-propylene glycol, 1, 5-pentanediol, neopentyl glycol, 1, 6-ethylene glycol, 3-methyl-1, 5-pentanediol, 1, 9-nonanediol, 2-ethyl-2-butyl-1, 3-propylene glycol, hydroxypivalic acid DOPCP, dihydroxymethyl heptane, 2, 2, 4-trimethylammonium-1, 3-pentanediol, 1, 4-cyclohexandiol, 1, 4-cyclohexanedimethanol, three ring decanediols, Tricyclodecane Dimethanol, at least one in volution ethylene glycol.
6. a kind of glue manufacture craft that is raw material with phthalic anhydride system polyvalent alcohol according to claim 1, is characterized in that: described antioxidant is antioxidant 264 or antioxidant 1010 or antioxidant 1076 or TPP or TNP.
7. a kind of glue manufacture craft that is raw material with phthalic anhydride system polyvalent alcohol according to claim 1, is characterized in that: described ultraviolet absorbers is UV-24 or UV-9 or Salol or OPS or BAD or UV-P or UV-236.
8. a kind of glue manufacture craft that is raw material with phthalic anhydride system polyvalent alcohol according to claim 1, is characterized in that: described catalyzer is dibutyl tin laurate or stannous octoate.
9. a kind of glue manufacture craft that is raw material with phthalic anhydride system polyvalent alcohol according to claim 1, is characterized in that: described environment-friendly type solvent be one or both and above combination in methylcarbonate, propylene carbonate, ethylene dimethyl, Methyl glutarate, succinic acid diformazan.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510646049.9A CN105153987A (en) | 2015-10-08 | 2015-10-08 | Process for producing glue by adopting phthalic anhydride series polyatomic alcohol as raw material |
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| CN201510646049.9A CN105153987A (en) | 2015-10-08 | 2015-10-08 | Process for producing glue by adopting phthalic anhydride series polyatomic alcohol as raw material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112226190A (en) * | 2020-09-30 | 2021-01-15 | 上海东睿化学有限公司 | Preparation method of moisture-curing polyurethane hot melt adhesive for textile compounding |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102732206A (en) * | 2012-07-04 | 2012-10-17 | 浙江多邦化工有限公司 | Environment-friendly polyurethane binder |
| US8822595B2 (en) * | 2008-08-28 | 2014-09-02 | Huntsman International Llc | Mixture obtained by reacting polyol and anhydride and its use in polyisocyanates for making polyisocyanurates |
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- 2015-10-08 CN CN201510646049.9A patent/CN105153987A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8822595B2 (en) * | 2008-08-28 | 2014-09-02 | Huntsman International Llc | Mixture obtained by reacting polyol and anhydride and its use in polyisocyanates for making polyisocyanurates |
| CN102732206A (en) * | 2012-07-04 | 2012-10-17 | 浙江多邦化工有限公司 | Environment-friendly polyurethane binder |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112226190A (en) * | 2020-09-30 | 2021-01-15 | 上海东睿化学有限公司 | Preparation method of moisture-curing polyurethane hot melt adhesive for textile compounding |
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Application publication date: 20151216 |