Waterborne polyurethane coating is one of the products with a large market demand . It is suitable for high and mid-range wood furniture ( furniture, etc. ) with a temperature-sensitive temperature lower than (60 - 80) °C at room temperature , and is used for high-grade architectural decoration, high-grade automobiles, Middle and surface coatings for aircraft and aerospace equipment.
   product ingredients:
   1. Modified trimer crosslinker products can be manufactured from isocyanates such as TDI , IPDI , MD I and XDI . The aromatic NCO reaction temperature is (120 - 150) °C and the aliphatic NCO reaction temperature is (150 - 200) °C. Its biggest advantage is no yellowing , water white and transparent , more suitable for carboxylic acid-based aqueous polyurethane crosslinking agent at room temperature. To enhance the overall performance, requires the use of two different reactive NCO groups diisocyanate, and produced in the reaction end want polyol NCO - acid reacted, to facilitate the neutralization and water-soluble amine product. Because of its high melting point, the reaction needs to be phased in an organic solvent, and an organic phosphine catalyst temperature above 120 deg.] C, the isocyanate may occur from the polycondensation reaction to produce a trimer compound. Pentyl phosphine catalyst heterocycle which hydrogen is the most effective, low reaction temperature, the yield up to 90%, then the catalytic trimerization promote completion of the reaction, and residues blocked.
   Product Formulation: NCO : Polyol carboxylic acid ( substance ratio ) of 6 : 1 : 1.43 .
   Process Steps : Preparation of polyol - carboxylic acid solution , neopentyl glycol, trimellitic anhydride, DMPA , xylene, and toluene are added into the reaction vessel and stirred according to the formula , and the temperature is raised to 80 °C . After the dissolution is complete , the temperature is raised to 148 °C. After being transparent , filter out the material for use. Imide prepolymer prepared: formulation will press xylene, toluene was added to the reaction vessel, heated to 148 deg.] C to reflux dehydration, addition of 10% phosphoric acid (in toluene) was cooled to 120 deg.] C, purged with nitrogen, the TD I, IPDI was added monomer dropping tank, after the completion of the dropwise over 2. 5h, the reaction temperature was raised to 130 ℃ IH, heterocyclyl pentyl phosphine 10% hydrogen was added to the kettle dropwise, slowly added dropwise, constantly observe the reactions of the material, to prevent After exploding , the reaction was completed at 130 °C for 2 h , 140 °C for 1 h , and 145 °C for 30 min. The temperature was lowered to 70 °C . The polyol - carboxylic acid solution was added dropwise to the dropping kettle . The reaction was completed at 70 °C ( 2-3). h, detection of NCO conversion rate of 96%, adding 10% lithium acetate solution , there are two processes : First, cooling to 25 °C , set aside for 7d; the second is to raise the temperature to (80 - 90) °C Reaction (2 - 3 h) Measure free TD I below 0.3% , add 10% methyl p-toluenesulfonate solution and 10% dimethylpyrazole solution to 85 °C for 20 min, and vacuum to remove 2/3 of the organic solvent . Add a hydrophilic solvent to adjust the solid content to 50%. Cool down to 50 °C. Add 50% aqueous triethylamine solution and N- toluene diethanolamine to adjust the p H value to 8.5. Raise the temperature to 60 °C . Warm to 40 °C discharge.
   2. Modified HDI Biuret Crosslinker
   product ingredients:
    NCO : H2O = 3 : 1.1 , NCO : OH = 6 : 1, Theoretical NCO content = 15.9%, using a staged polymerization reaction, neutralization method.
   Process Steps : Preparation of polyol - carboxylic acid solution , neopentyl glycol, trimellitic anhydride, DMPA , xylene, and toluene were added to the reaction kettle according to the formula , heated to 80 °C and dissolved uniformly , and then heated to 148 °C. After being transparent and dry , it is cooled down to 40 °C and used for discharging. Preparation of HDI prepolymer : According to the formula, diisocyanate and xylene are added into the reaction vessel , nitrogen is introduced , the temperature is raised to 65 ° C. , 10% phosphoric acid ( toluene ) solution is added , and the deionized water is added to the dropping kettle to start dropping. , The reaction is self-heating , and the self-heating temperature is controlled below 80 °C . After completion of the dropwise addition , the temperature is increased to 90 °C for 1 h , 120 °C for 2 h , and 130 °C for 1 h, and the temperature is lowered to 70 °C . The polyol - carboxylic acid solution is added dropwise. kettle dropwise addition was added dropwise to the reaction at 70 ℃ (2 - 3) h , 80 ℃ 1h, the measured free HDI <0.2%, the organic solvent was evacuated prolapse, a hydrophilic solvent is added to adjust the solid content of 50%, cooled to 50 Add 50% triethylamine aqueous solution at °C , adjust the p H value of 8.4, warm up to 60 °C, react to be transparent , cool to 40 °C, filter and discharge.
 3. Modified TD I Trimer Crosslinker
   Product formula :
   NCO : OH ( amount ratio of the substance ) is 6 : 1, using trimerization catalytic reaction, termination reaction, residue blocking method and phased reaction.
   Process Step: Polyol - carboxylic acid solution, formulated trimethylol propane, neopentyl glycol, trimellitic anhydride, DM - PA, butyl acetate, xylene was added was stirred reactor heated to 80 deg.] C Dissolve it evenly , and then heat it up to 148 °C. Dehydrate it to reflux and make it transparent . Cool it to 40 °C and filter it out for use.
   Trimer Preparation: According to recipe xylene, toluene was added to the reaction kettle with stirring, warmed to 148 ℃ After removal of water at reflux, cooled to 120 deg.] C, 10% phosphoric acid was added lithium mix, nitrogen, the monomer was added dropwise TDI The kettle was added dropwise . After 3 hours of addition , the reaction was incubated at 120 °C for 2 hours and at 130 °C for 1 hour. The temperature was lowered to 65 °C . The polyol - carboxylic acid solution was added dropwise to the dropping kettle . The reaction was self-heating and the temperature was controlled. Below 75 °C , dropping , 80 °C insulation 2h, sampling free TDI < 0.9%, adding 10% phosphoric acid toluene solution heated to 85 °C reaction for 2h ( or to 25 °C for 7d), detection of free TDI < 0.2%, Add 10% dimethyl sulphate solution and 10% dimethylpyrazole solution to 90 °C to react for 15min. Vacuum to remove organic solvent . Add hydrophilic solvent to adjust solid content to 50%. Cool down to 50 °C. Add 50% The aqueous amine solution and N- toluene diethanolamine adjusted the p H value to 8.4 and heated up to 60 °C. The reaction was transparent and the temperature was lowered to 40 °C.
   4, TD I / TMP addition, modified crosslinker
   Product formula :
   NCO : OH ( amount ratio of the substance ) is 3 : 1, using a trimerization catalytic reaction, termination reaction, and residue blocking method. Process Step: Polyol - carboxylic acid solution, the formulation according to the TMP, neopentyl glycol, trimellitic anhydride, of DMPA, butyl acetate was added with stirring reactor was heated to 80 deg.] C to dissolve uniformly, heated to 140 deg.] C to a reflux dehydrator Transparent , cooled to 40 °C , filtered out for use.
   Adduct preparation : According to the formula, butyl acetate and toluene are added to the reaction vessel to stir and warm up to 140 °C. After dehydration at reflux , the temperature is lowered to 60 °C. TDI is added , nitrogen is introduced , and the polyol - carboxylic acid solution is added to the dropping kettle to start dropping. The reaction was self-heating and the addition was slow . The temperature was controlled to drop below 70 °C . 10% phosphoric acid toluene was added and the reaction was carried out at 70 °C (4-5 hours) . Detection of NCO content of 13.1%, free TDI at 12.5%, adding 10% tri-n-butyl phosphine liquid stir , heated to 85 °C reaction ( 2-3) h ( or cooled to 25 °C , set aside for 7d), sampling test Free TDI < 0.2%, add 10% benzoyl chloride solution, 10% dimethylpyrazole solution heated to 90 °C , the reaction 15min, vacuum decompression , remove the organic solvent , add hydrophilic solvent , adjust the solid content 50%, Cool down to 50 °C, add 50% triethylamine aqueous solution, N- toluene diethanolamine to adjust the p H value of 8.5, warm up to 60 °C. The reaction is transparent and cool to 40 °C.
   5. XDI/ TMP addition modifier , NCO crosslinker
   Product formula :
   NCO:OH ( amount ratio of material ) = 9:1, using trimerization, termination, and residue blocking.
   Process step : Refer to the fourth process step.
   6 , modified TD I alcohol oil , NCO cross-linking agent
   Product formula :
   Oil 86.4 %, K = 0.93, alcohol excess R = 1.17, NCO: 1OH ( volume ratio of substance ) = 3: ( containing hydroxyl groups in castor oil ), trimerization, termination, and residue blocking.
   Process Step : Add TD I , castor oil, and neopentyl glycol to the reaction vessel according to the formula , increase the temperature to 120 °C, add calcium naphthenate , stir and heat up to 240 °C , alcoholyze the reaction (2-3 h), and sample and test the sample. Transparency , after the pass, the temperature is lowered to 180 °C , benzene triacetic anhydride is added, DMPA is reacted for 40 min, cooled to 120 °C, diluted with toluene , heated up to 134 °C, refluxed and dehydrated , the water is dehydrated , the temperature is lowered to 60 °C , and TDI is added dropwise , 2h Dripping , adding 10% phosphoric acid to toluene, stirring , heating to 70 °C reaction ( 3-4) h, test NCO content of 12% , free TDI at 9.5%, add 10% alkyl phosphine solution, stir , warming to 80 °C reaction ( 2-3) h ( or cool down to 25 °C for 7 days), test free TDI < 0.3%, add 10% benzoyl chloride solution, 10% dimethylpyrazole solution, stir and heat to 90 °C, react for 15 minutes pumping all the toluene in vacuo under reduced pressure extrusion, a hydrophilic solvent is added to adjust the solid content of 50%, cooled to 50 deg.] C was added triethylamine, N - toluene diethanolamine, adjust p H value of 8.5, the reaction temperature was raised to 60 deg.] C to the clear , cool down to 40 °C filter , discharge.
   7, water-based polyester polyurethane
   Product formulation ( Part A ): OH : NCO ( substance ratio ) = 1.5:1, K = 1.02, alcohol excess R = 1.18 .
   Process steps : According to the formula, neopentyl glycol, adipic acid, trimellitic anhydride and DMPA are added into the reaction vessel , CO2 gas is introduced , the temperature is raised to 120 ° C. , tetraisopropyl titanate is added , and the temperature is raised to 180 ° C. with stirring . after the reaction 2h, every 30min acid number of samples tested, until 79mg KOH / g, a hydroxyl value of 79.5, was added to cool to 130 ℃ xylene heated to 150 deg.] C to reflux dehydrated, Tuojin, vacuum xylene recovery, Cool down to 80 °C, dilute with acetone , incubate at 60 °C for 1.5 h , add TDI dropwise , add 10% phosphoric acid ( toluene ) solution, mix well , heat up to 70 °C for reaction ( 4-5)h, test free TDI < 0.2 %, add 50% phenol ( toluene ) solution heated to 80 °C reaction 15min, and then heated to 90 °C , distilled 1/2 charge amount of acetone , 70 °C insulation standby. In another reactor equipped with rapid stirring, toluene was added N- diethanolamine, triethylamine, ethylenediamine, start of deionized water with rapid stirring, to the above-described insulation material at 70 deg.] C, the reactor was slowly added, at 60 °C Neutralization reaction was carried out after the transparent , heated to 70 °C , vacuum decompression , distillation of the remaining acetone , cooled to 40 °C , filtered and discharged.
   8, water-based soybean oil polyester polyurethane
   Product formulation ( Part A ): OH : NCO ( substance ratio ) = 1:1.5, resin K = 1.019, alcohol excess R = 1.3 , r = 1.5, oil content 56% .
   Process Step: Soybean oil fatty acid according to the formula, castor oil fatty acid, pentaerythritol, neopentyl glycol into a reactor, into CO 2 gas, heated to 120 deg.] C was added dibutyltin dilaurate was stirred and heated to 220 deg.] C, the reaction 3h, 180 [deg.] C was added cooling to room acid, trimellitic anhydride, reacted at 180 [deg.] C of DMPA after 2h, the test samples every 30min its acid value, until 75mg KOH / g, a hydroxyl value of 80, cooling to 120 deg.] C was added toluene was heated to reflux for 132 ℃ dehydrated, Tuojin, cooled to 65 deg.] C was added a 10% solution of phenol in toluene mix, the TDI was added dropwise a monomer kettle dropwise addition, the dropwise addition for 1.5 h, the reaction was warmed to 70 deg.] C 4h, 80 °C lh, test free TDI 0.2%, add 50% phenol ( toluene ) solution and stir , heat to 90 °C for 15min, vacuum decompression to remove 2/3 of toluene , add isobutanol to cool down to 50 °C , triethylamine, ethanolamine and xylene 1/3 deionized water, adjust p H value of 8.6, the reaction was heated to 60 deg.] C to a transparent, all vacuum extrusion toluene, add the remaining deionized water, adjusting the solid content 50 %, filter , discharge.
   9 , water-based vegetable oil alkyd polyurethane
   Product formulation ( Part A ): OH : NCO ( mass ratio of substance ) = 1:1.5, resin K value = 1.01, alcohol excess R = 1.314, r = 1.499, oil content = 55.2%, theoretical NCO content = 228 % .
   Process steps: the rapeseed according to formula (salad) oil, castor oil fatty acid, TMP, neopentyl glycol into a reactor, into CO2 gas, heated to 120 deg.] C was added lithium naphthenate stirring, the reaction temperature was raised to 230 deg.] C (2 ~ 3) h, after passing the test alcoholysis transparent, cooled to 180 ℃, was added phthalic anhydride, trimellitic anhydride, of DMPA, after 2h the reaction at 180 ℃, every 30min, a test acid value 70mg KOH until / g up, then cooled to 110 deg.] C was added toluene and heated to 132 deg.] C dehydrated, after Tuojin water, cooled to 65 deg.] C was added 10% phosphoric acid (in toluene) was homogenized, the TDI was added dropwise a monomer vessel, began to drop was added dropwise after the temperature was raised to 70 deg.] C the reaction (4 - 5) h, 80 ℃ 1h, test 0.2% free TDI, was added 50% phenol (toluene) solution, the reaction temperature was raised to 90 deg.] C 15min, vacuum prolapse 1/3 toluene, was added isopropyl alcohol, cooling to 50 deg.] C was added N - dimethylethanolamine, triethylamine, and 1/2 of deionized water, adjust the p H value of 8.6, the reaction was heated to 60 deg.] C to the clear, vacuum Remove all the toluene , add the remaining deionized water , adjust the solid content 50%, filter , discharge.
   10 , water-based castor oil alkyd polyurethane
   Product formula ( Part A ): OH : NCO ( substance ratio ) =1 : 1.5, resin K value = 0197, alcohol excess R = 1.23, r = 1.36, oil content = 5514%, theoretical NCO content = 2.3 % .
   Process steps: according to the formula castor oil, glycerol (95%), neopentyl glycol into a reactor, into CO2 gas, heated to 120 deg.] C was added lead oxide was stirred and heated to 230 deg.] C, the reaction (2-3) h after passing tested alcoholysis transparent, cooling to 180 [deg.] C was added phthalic anhydride, trimellitic anhydride, of DMPA, rosin diol, the reaction after 2h 180 ℃, every 30min test acid value, until 80mg KOH / g , then cooled to 110 °C to add toluene , heated to 128 reflux dehydration , after detoxification , adding 10% phosphoric acid toluene solution was cooled to 65 °C , with 1.5h finished TDI, heated to 70 °C reaction 4h, 80 °C 1h, The free TDI was tested to 0.2%, 50% phenol ( toluene ) solution was added , and the temperature was raised to 95. The reaction was carried out for 15 minutes. Vacuum was used to remove 1/2 amount of toluene , isopropyl alcohol was added , and the temperature was decreased to 50 to add monoethanolamine, triethylamine and 1 /2 amount of deionized water , adjust the pH value to 8.6, warm up to 60 °C, react to be transparent , remove all toluene by vacuum , add the remaining deionized water , filter and discharge.
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