CN102443308A - Preparation method for epoxy floor paint curing agents - Google Patents
Preparation method for epoxy floor paint curing agents Download PDFInfo
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- CN102443308A CN102443308A CN201010509268XA CN201010509268A CN102443308A CN 102443308 A CN102443308 A CN 102443308A CN 201010509268X A CN201010509268X A CN 201010509268XA CN 201010509268 A CN201010509268 A CN 201010509268A CN 102443308 A CN102443308 A CN 102443308A
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Abstract
The invention relates to the field of building paint, in particularly to a preparation method for epoxy floor paint curing agents. Adopted raw materials comprise 15 percent to 25 percent of diphenylmethane diisocyanate, 1 percent to 3 percent of trimethylolpropane, 10 percent to 20 percent of polyether polyol and 55 percent to 65 percent of dimethylbenzene. The method comprises the following steps that: 1, the dimethylbenzene accounting for 2 percent to 10 percent of the total weight of the raw materials is taken and is mixed with the diphenylmethane diisocyanate and the polyether polyol, the materials are heated, the heating is stopped when the temperature is raised to 50 to 55 DEG C; 2, the trimethylolpropane is added when the temperature is raised to 58 to 62 DEG C; 3, the temperature is controlled at 66 to 72 DEG C, and the reaction lasts 3 to 6 hours; 4, after the reaction is completed, the rest dimethylbenzene is added in the temperature reduction process, and the materials are uniformly mixed; and the filtering and the packing are carried out when the temperature is 32 to 40 DEG C, and the epoxy floor paint curing agents are obtained. The diphenylmethane diisocyanate is used for replacing the toluene diisocynate, the harm to human bodies and the environment can be reduced during the production and the use, and the performance of the product is good.
Description
Technical field
The present invention relates to the trade sales coating field, be specially a kind of preparation method of epoxide terrace paint solidifying agent.
Background technology
Traditional epoxide terrace paint generally comprises first component and component B, and component B comprises resin and solvent, and the first component is generally solidifying agent and solvent; During use first component and component B are mixed by a certain percentage, the first component also can use separately.
The epoxide terrace paint first component that circulates on the home market at present; The preparation method is: with tolylene diisocyanate (TDI), TriMethylolPropane(TMP) (TMP), polyether glycol (like GE-210 etc.) and YLENE (xylol) is starting material, makes polyurethane prepolymer through two step method or film evaporation method.Though these two kinds of methods can be reduced to the TDI of free state below 0.5%, owing to the existence of TDI, still entail dangers to is to HUMAN HEALTH when construction and production.In environmental protection and health requirements increasingly high today, user and manufacturer all hope to find a surrogate to substitute TDI or develop a new product to substitute existing first component.
Summary of the invention
The present invention aims to provide a kind of preparation method of epoxide terrace paint solidifying agent.
Technical scheme does, a kind of preparation method of epoxide terrace paint solidifying agent, and raw material comprises:
Diphenylmethanediisocyanate (MDI) 15%～25%,
TriMethylolPropane(TMP) (TMP) 1%～3%,
Polyether glycol 10%～20%
YLENE 55%～65%,
Above-mentioned raw materials per-cent all is weight percentage; And in the above-mentioned raw materials, the NCO/OH of diphenylmethanediisocyanate and TriMethylolPropane(TMP) is 1～2;
Preferably, raw material weight per-cent is:
Diphenylmethanediisocyanate (MDI) 17%～23%,
TriMethylolPropane(TMP) (TMP) 1%～2%,
Polyether glycol 15%～18%
YLENE 58%～65%;
The polyether glycol hydroxyl value is 50～150 mg KOH/g;
Described polyether glycol molecular weight is 800～2200, and prepolymer is divalent alcohol or trivalent alcohol;
Preparation process comprises:
(1) get the YLENE of raw material gross weight 2%～10%, under agitation add diphenylmethanediisocyanate and polyether glycol and mix, heating, temperature stops heating when rising to 50～55 ℃;
(2) treat to add when temperature rises to 58～62 ℃ TriMethylolPropane(TMP);
(3) temperature was controlled between 66～72 ℃ sustained reaction 3～6 hours;
(4) after reaction finishes, add remaining diformazan benzo mixing in the temperature-fall period; When temperature is reduced to 32～40 ℃, filter and package, obtain the epoxide terrace paint solidifying agent.
Raw material also can comprise 0.1% ~ 0.2% auxiliary agent, and the kind of auxiliary agent comprises skimmer and oxidation inhibitor.Auxiliary agent finishes the back in reaction and adds.
The present invention utilizes '-diphenylmethane diisocyanate (MDI) to substitute tolylene diisocyanate (TDI); With the epoxide terrace paint solidifying agent (first component) that TriMethylolPropane(TMP), polyether glycol and YLENE make through two step method, each item performance satisfies the use of epoxide terrace; Concrete surface (manufacturing building and the workshop and the warehouse of food, medicine, chemical industry, tobacco, electrical equipment, electronics or machinery, parking and hypermarket etc.) applicable to all kinds of interior of buildings; Can reach seamless dust-proof effect, good decorating effect, strong adhesion, snappiness and wear resistance are good, and be easy to clean, anti-general chemical corrosion, the life-span is lasting.When producing and use, reduce the harm of human body and reduce pollution environment.
Embodiment
Embodiment 1
Raw material comprises: diphenylmethanediisocyanate (MDI) 20.5kg, TriMethylolPropane(TMP) (TMP) 1.7kg, polyether glycol GE-210 (molecular weight is 1000 divalent alcohol polymkeric substance) 16.6kg, YLENE 61.2kg.
MDI purity is more than 99.5%, and 2,2 ,-MDI content≤0.8%, 2,4 ,-MDI content 50 ± 5%; Polyether glycol GE-210 hydroxyl value 107-117mg KOH/g, acid number≤0.08 mgKOH/g, pH value 5～7, moisture≤0.05%;
The NCO/OH of diphenylmethanediisocyanate and TriMethylolPropane(TMP) is 1～2.
Reactions step is:
(1) gets 10kg YLENE, drop in the reaction kettle, start stirring; And with MDI and polyether glycol GE-210 input reaction kettle, heating, temperature stops heating when rising to 52 ℃;
(2) treat that temperature rises to 60 degree ℃ adding TMP;
(3) temperature is controlled at 70 ± 2 between sustained reaction 4.5 hours;
(4) after reaction finishes, when reducing to 60 ℃ of left and right sides, temperature adds residue diformazan benzo mixing; When temperature is reduced to 35 ℃, filter and package, obtain epoxide terrace paint solidifying agent (first component).
Resulting product detected result such as table 1, the toxicity of MDI and TDI are relatively like table 2:
Table 1
| Project and standard | Detected result |
| Pencil hardness (scratch) >;=H | 2H |
| Sticking power (drawing compartment)<=1 apart from 1mm | 0 grade |
| Shock-resistance | The 50cm permission slight deformation that do not come off that do not ftracture |
| Snappiness<=2mm | 1mm |
| Wear resistance (750g/500r)<=0.060g | 0.013g |
| Water tolerance (7d) | Non-foaming, do not come off, allow light discolouration |
| Oil-proofness (120# gasoline, 7d) | Non-foaming, do not come off, allow light discolouration |
| Acid resistance (10%H 2SO 4，48h） | Non-foaming, do not come off, allow light discolouration |
| Alkali resistance (100g/LNaOH, 48h) | Non-foaming, do not come off, allow light discolouration |
| Resistance to salt water (30g/LNaCl, 7d) | Non-foaming, do not come off, allow light discolouration |
Table 2
| ? | TDI | MDI |
| The oral median lethal dosage LD of rat 50? g/kg | TDI（80/20）? 1.95-5.8 | 31.6 |
| Suck median lethal dosage LD through skin 50 G/kg (rabbit) | TDI (2,4 body) 16 | 10 |
| To ocular injury | Seriously | Seriously |
| Vp (25 ℃) | 3.3Pa | 0.012Pa |
Detected result shows, replaces with MDI that each item performance index of product reach request for utilization behind the TDI, and do not contain the TDI of any free state, when producing and use, reduces the harm to human body.
Embodiment 2
Raw material comprises: diphenylmethanediisocyanate (MDI) 18.6kg, TriMethylolPropane(TMP) (TMP) 1.4kg, polyether glycol GE-210 15.6kg, YLENE 64.2kg, each 0.1kg of skimmer and inhibitor.The NCO/OH of diphenylmethanediisocyanate and TriMethylolPropane(TMP) is 1～2.
Reactions step is:
(1) gets 5kg YLENE, drop in the reaction kettle, start stirring; And with MDI and polyether glycol GE-210 input reaction kettle, heating, temperature stops heating when rising to 52 ℃;
(2) treat that temperature rises to 62 ℃ and adds TMP;
(3) temperature was controlled between 70 ± 2 ℃ sustained reaction 4 hours;
(4) after reaction finishes, when reducing to 60 ℃ of left and right sides, temperature adds residue YLENE and skimmer and inhibitor and mixing; When temperature is reduced to 35 ℃, filter and package, obtain the epoxide terrace paint solidifying agent.Detected result reaches the standard of table 1.
Embodiment 3
Raw material comprises: diphenylmethanediisocyanate (MDI) 22.4kg, and TriMethylolPropane(TMP) (TMP) 2.0kg, (molecular weight is 2000 divalent alcohol polymkeric substance to polyether glycol PPG-2000; Hydroxyl value 54～58 mg KOH/g; Acid number≤0.05 mg KOH/g, pH value 5～7, moisture≤0.05%) 17.5kg; YLENE 58kg, each 0.05kg of skimmer and inhibitor.The NCO/OH of diphenylmethanediisocyanate and TriMethylolPropane(TMP) is 1～2.
Reactions step is:
(1) gets 4kg YLENE, drop in the reaction kettle, start stirring; And with MDI and polyether glycol GE-210 input reaction kettle, heating, temperature stops heating when rising to 50 ℃;
(2) treat that temperature rises to 60 ℃ and adds TMP;
(3) temperature was controlled between 68 ± 2 ℃ sustained reaction 5 hours;
(4) after reaction finishes, when reducing to 60 ℃ of left and right sides, temperature adds residue YLENE and skimmer and inhibitor and mixing; When temperature is reduced to 35 ℃, filter and package, obtain the epoxide terrace paint solidifying agent.Detected result reaches the standard of table 1.
Claims (5)
1. the preparation method of an epoxide terrace paint solidifying agent is characterized in that, raw material comprises:
Diphenylmethanediisocyanate 15%～25%,
TriMethylolPropane(TMP) 1%～3%,
Polyether glycol 10%～20%
YLENE 55%～65%,
Above-mentioned per-cent all is weight percentage;
Preparation process comprises:
(1) get the YLENE of raw material gross weight 2%～10%, under agitation add diphenylmethanediisocyanate and polyether glycol and mix, heating, temperature stops heating when rising to 50～55 ℃;
(2) treat to add when temperature rises to 58～62 ℃ TriMethylolPropane(TMP);
(3) temperature was controlled between 66～72 ℃ sustained reaction 3～6 hours;
(4) after reaction finishes, add remaining diformazan benzo mixing in the temperature-fall period; When temperature is reduced to 32～40 ℃, filter and package, obtain the epoxide terrace paint solidifying agent.
2. the preparation method of claim 1 or 2 said a kind of epoxide terrace paint solidifying agent is characterized in that, described raw material weight per-cent is:
Diphenylmethanediisocyanate (MDI) 17%～23%,
TriMethylolPropane(TMP) (TMP) 1%～2%,
Polyether glycol 15%～18%
YLENE 58%～65%.
3. the preparation method of claim 1 or 2 said a kind of epoxide terrace paint solidifying agent is characterized in that, the NCO/OH of described diphenylmethanediisocyanate and TriMethylolPropane(TMP) is 1～2.
4. the preparation method of claim 1 or 2 said a kind of epoxide terrace paint solidifying agent is characterized in that, described polyether glycol hydroxyl value is 50～150 mg KOH/g, and molecular weight is 800～2200, and prepolymer is divalent alcohol or trivalent alcohol.
5. the preparation method of claim 1 or 2 said a kind of epoxide terrace paint solidifying agent is characterized in that, raw material also comprises the auxiliary agent of 0.1% ~ 0.2% weight ratio, and the kind of auxiliary agent is skimmer and oxidation inhibitor, and auxiliary agent finishes the back in step (4) reaction and adds.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010509268XA CN102443308A (en) | 2010-10-15 | 2010-10-15 | Preparation method for epoxy floor paint curing agents |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010509268XA CN102443308A (en) | 2010-10-15 | 2010-10-15 | Preparation method for epoxy floor paint curing agents |
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| Publication Number | Publication Date |
|---|---|
| CN102443308A true CN102443308A (en) | 2012-05-09 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201010509268XA Pending CN102443308A (en) | 2010-10-15 | 2010-10-15 | Preparation method for epoxy floor paint curing agents |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104910674A (en) * | 2015-06-17 | 2015-09-16 | 牛无畏 | Curing agent with high density and strong adhesive force and preparation method of curing agent |
| CN107880249A (en) * | 2017-11-24 | 2018-04-06 | 鹤山市信兴化工有限公司 | A kind of polyurethane curing agent and preparation method thereof |
| CN111484598A (en) * | 2020-04-14 | 2020-08-04 | 中国铁道科学研究院集团有限公司铁道建筑研究所 | High-strength single-component tunnel lining structure protective coating |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4832104B1 (en) * | 1967-08-07 | 1973-10-04 | ||
| JPH0832104B2 (en) * | 1990-06-21 | 1996-03-27 | 松下電器産業株式会社 | Speaker system |
| CN101230124A (en) * | 2007-01-27 | 2008-07-30 | 周建明 | Curing agent 4,4'-biphenyl methane diisocyanate prepolymer and preparation method thereof |
-
2010
- 2010-10-15 CN CN201010509268XA patent/CN102443308A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4832104B1 (en) * | 1967-08-07 | 1973-10-04 | ||
| JPH0832104B2 (en) * | 1990-06-21 | 1996-03-27 | 松下電器産業株式会社 | Speaker system |
| CN101230124A (en) * | 2007-01-27 | 2008-07-30 | 周建明 | Curing agent 4,4'-biphenyl methane diisocyanate prepolymer and preparation method thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104910674A (en) * | 2015-06-17 | 2015-09-16 | 牛无畏 | Curing agent with high density and strong adhesive force and preparation method of curing agent |
| CN107880249A (en) * | 2017-11-24 | 2018-04-06 | 鹤山市信兴化工有限公司 | A kind of polyurethane curing agent and preparation method thereof |
| CN111484598A (en) * | 2020-04-14 | 2020-08-04 | 中国铁道科学研究院集团有限公司铁道建筑研究所 | High-strength single-component tunnel lining structure protective coating |
| CN111484598B (en) * | 2020-04-14 | 2022-03-08 | 中国铁道科学研究院集团有限公司铁道建筑研究所 | High-strength single-component tunnel lining structure protective coating |
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| PB01 | Publication | ||
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| RJ01 | Rejection of invention patent application after publication | ||
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Application publication date: 20120509 |