十大水性聚氨酯涂料配方大揭密（Ten water polyurethane coating formula revealed）

1、十大水性聚氨酯涂料配方大揭密（Ten water polyurethane coating formula revealed）Ten water polyurethane coating formula revealed2007/8/30/09:14Recommended waterborne polyurethane coating is one of the products of larger market demand at present, it is suitable for heat sensitive temperature below (60 - 80) C crosslin

2、king at normal temperature is high, mid-range wood (furniture), high-grade building decoration, senior automotive, aircraft and aerospace equipment such as coating and surface coating.Product formula:1. The modified trimer crosslinking agent can be made from isocyanate such as TDI, IPDI, MD, I and X

3、DI. The aromatic NCO reaction temperature is (120 - 150) DEG C, and the reaction temperature of aliphatic NCO is (150 - 200) DEG C. It has the greatest advantages of no yellowing, clear white water, suitable for aqueous polyurethane such as carboxylic acids and so on. In order to enhance the overall

4、 performance, two NCO groups with different activity groups should be used, and the end NCO produced in the reaction will be reacted with polyol carboxylic acid to facilitate the neutralization of amines and the water solubility of the products. Because of its high melting point, the reaction needs

5、to be carried out in organic solvents in different stages. The organic phosphine catalyst and temperature above 120 degrees of temperature can lead to self polycondensation reaction of isocyanate and form trimer compound. The phosphine is the most effective catalyst in the catalyst. The reaction tem

6、perature is low and the yield is up to 90%. The reaction is completed by the catalytic method and the residue is closed.Product formula: NCO: polyol carboxylic acid (material ratio) is 6:1:1.43.Process steps: polyol - carboxylic acid solution preparation, the neopentyl glycol, benzene anhydride, par

7、tial DMPA, xylene, toluene added to the reactor mixing according to the formula, is heated to 80 DEG C, complete dissolution, heated to 148 DEG C reflux dehydration to transparent, filter material reserve. 亚胺预聚体的制备: 按配方将二甲苯、甲苯加入反应釜, 升温至148 回流脱水后, 加入10 % 磷酸( 甲苯) 液降温至120 , 通入氮气, 将TD I 、IPDI 加入单体滴加釜, 在

8、2 . 5h 内完成滴加后, 升温至130 反应1h , 将10 % 戊杂环膦化氢液加入滴加釜, 开始缓慢滴加, 不断观察物料反应情况, 防止爆聚, 滴完在130 反应2h 、140 1h 、145 30min , 降温至70 , 将多元醇- 羧酸液加入滴加釜开始滴加,滴完在70 反应(23) h , 检测NCO 转化率达96 % , 加入10 % 醋酸锂液, 此时有两种工艺: 一是降温至25 , 静置7d ; 二是升温至(8090) 反应(23) h , 测游离TD I 在0.3% 以下, 加入10 % 对甲苯 Two methyl sulfonate solution and 10% me

9、thyl pyrazole liquid is heated to 85 DEG C 20min, organic solvent, vacuum pumping off the 2/3 volume, adding hydrophilic solvent regulating solid content is 50%, down to 50 deg.c 50% three triethylamine aqueous solution and N- toluene two ethanol amine to adjust P H value to 8.5, heating to 60 DEG C

10、 to transparent, cooling to 40 DEG C discharge.2. Modified HDI shrinkage two urea crosslinking agentProduct formula: NCO:H2O = 3:1.1, NCO:OH =6:1, theoretical NCO content = 15.9%, using stage polymerization and neutralization.Process steps: polyol - carboxylic acid solution was prepared according to

11、 the formula, the neopentyl glycol, trimellitic anhydride, DMPA, xylene, toluene is added into the reaction kettle is heated to 80 DEG C, uniform dissolution, and then heated to 148 DEG C reflux dehydration to transparent anhydrous after cooling to 40 DEG C material reserve. HDI prepolymer preparati

12、on: prepared with hexamethylene diisocyanate and xylene into reactor, adding nitrogen, heated to 65 DEG C, adding 10% phosphoric acid (toluene) liquid mix, adding deionized water into the kettle began dropping, exothermic reaction, control self heating at 80 DEG C, complete drop after heating the re

13、action of 1H to 90 DEG C and 120 C, 130 C 2H 1H, cooling to 70 DEG C, the polyol carboxylic acid solution into the dropping kettle began dropping,After drops in 70 DEG C (2 - 3) h, 80 degrees 1H, detecting free HDI 0.2%, vacuum from the organic solvent, adding hydrophilic solvent, adjusting the soli

14、d content of 50%, down to 50 deg.c 50% aminoethane solution of three P, H value 8.4, heating to 60 DEG C reaction to transparent. Cooling to 40 DEG C filter material.3. Modified TD I trimer crosslinkerProduct formula: NCO:OH (material ratio) of 6:1, using trimeric catalytic reaction, termination rea

15、ction, residue sealing method and stage reaction.Process steps: polyol - carboxylic acid solution was prepared according to the formula, three hydroxymethyl propane, neopentyl glycol, trimellitic anhydride, DM - PA, butyl acetate, xylene into reactor stirring, heating to 80 Deg. C dissolved, and the

16、n heated to 148 DEG C to the refluxing temperature drop to transparent. 40 C filter material reserve.Preparation: according to the formula the trimerization of xylene and toluene are added into a reaction kettle for stirring and heating to 148 DEG C reflux off the water after cooling to 120 DEG C, a

17、dding 10% lithium phosphate liquid nitrogen, stir well, add TDI monomer dripping kettle began to drop, 3h drops after adding insulation, 2h, 120 DEG C 130 DEG 1H, cooling to 65 DEG C, the polyol carboxylic acid solution into the dropping kettle dropping, exothermic reaction, temperature controlled a

18、t 75 DEG C, drop, 80 DEG C 2H, sampling measurement of free TDI 0.9%, adding 10% phosphoric acid toluene liquid is heated to 85 DEG C to 25 C (or reaction of 2H static 7D), detection of free TDI 0.2%, add 10% two, 10% two methyl sulfate liquid methylpyrazole liquid is heated to 90 DEG C 15min, vacuu

19、m pumping out organic solvent, adding hydrophilic solvent to regulate solid content to 50%, down to 50 deg.c 50% three triethylamine aqueous solution and N toluene Two ethanolamine regulates P, H value is 8.4, heating up to 60 DEG C, reaction to transparent, cooling down to 40 DEG C discharging.4, T

20、D, I/, TMP addition, modifier crosslinking agentProduct formula: NCO:OH (material ratio) of 3:1, using trimeric catalytic reaction, termination reaction, residue sealing method. Process steps: polyol - carboxylic acid solution preparation, TMP, neopentyl glycol, benzoic anhydride, partial DMPA, buty

21、l acetate is added into the reaction kettle is heated to 80 DEG C stirring evenly dissolved according to the formula, heating to 140 DEG C reflux dehydration to transparent, cooling to 40 DEG C, filtering material reserve.Adduct was prepared according to the formula: the butyl acetate and toluene in

22、 the reactor is heated to 140 DEG C stirring reflux after dehydration, cooling to 60 DEG C to join TDI, adding nitrogen, the polyol carboxylic acid solution into the dropping kettle dropping, reaction heat, dripping slowly, temperature controlled at 70 DEG C to under the drop, adding 10% phosphoric

23、acid toluene solution, reacting at 70 DEG C (4 - 5) H. Detection of NCO content of 13.1%, free TDI in 12.5%, adding 10% tributyl phosphine liquid mixture is heated to 85 DEG C reaction (2 - 3) H (or cooling to 25 DEG C, static 7D), sampling detection of free TDI 0.2%, adding 10% benzoyl chloride sol

24、ution, 10% methyl pyrazole liquid is heated to two 90 C, reaction 15min, vacuum pressure, from organic solvent, adding hydrophilic solvent, adjusting the solid content of 50%, down to 50 deg.c 50% three triethylamine aqueous solution, two ethanol N- toluene amine to adjust p value of H was 8.5, the

25、reaction temperature is raised to 60 DEG C to transparent, cooling to 40 DEG C filter material.5, XDI / TMP addition modifier, NCO crosslinkerProduct formula: NCO:OH (material ratio) = 9:1, using trimeric catalysis, termination, residue sealing method.Process steps: refer to fourth process steps.6,

26、the modified TD I alcoholysis oil, NCO crosslinking agentProduct formula: oil 86.4%, K = 0.93, alcohol excess R = 1.17, NCO:1OH (material ratio) = 3: (containing hydroxyl in castor oil), using trimeric catalysis, termination, residue sealing method.Process steps: TD, I, castor oil and new glycol are

27、 added into the reaction kettle according to the formula,The temperature to 120 deg.c calcium naphthenate, stirring and heating to 240 DEG C, alcoholysis reaction (2 - 3) h, sampling and testing its transparency, qualified after cooling to 180 DEG C, adding Benzene Partial anhydride and DMPA reactio

28、n of 40min, cooling to 120 DEG C with toluene dilution, heating to 134 DEG C reflux dehydration, water removal after all, cooling to 60 DEG C, dropping TDI, 2h drop, adding 10% phosphoric acid toluene liquid mixture is heated to 70 DEG C reaction (3 - 4) H test, NCO content in 12%, free TDI in 9.5%,

29、 adding 10% alkylphosphonate liquid mix is heated to 80 DEG C reaction (2 - 3) H (or cooling to 25 DEG 7d, static test free) TDI 0.3%, adding 10% benzoyl chloride solution, 10% two methyl pyrazole liquid mix is heated to 90 DEG C 15min, vacuum pressure from all toluene, adding hydrophilic solvent, a

30、djusting the solid content is 50%, down to 50 deg.c, three triethylamine N - methyl benzene two Ethanolamine is adjusted by P, H value is 8.5, heating up to 60 DEG C, reaction to transparent, cool down to 40 DEG C, filtered and discharged.7 、 waterborne polyester polyurethaneThe product formula (gro

31、up A): OH: NCO (molar ratio) = 1.5:1, K = 1.02, R = 1.18 in excess of alcohol.Process steps: neopentyl glycol, adipic acid, benzene anhydride, DMPA is added into a reaction kettle according to the formula, the CO2 gas is heated to 120 DEG C, adding four isopropyl titanate ester, mixing is heated to

32、180 DEG C, the reaction after 2h, every 30min sampling and testing its acid value, until it reached 79mg KOH/ g, hydroxyl value at 79.5, down to 130 deg.c xylene, heated to 150 DEG C reflux dehydration, Tuojin, vacuum recovering xylene, cooled to 80 DEG C adding acetone diluted, holding at 60 degree

33、s, 1.5h and TDI, after adding 10% drops of phosphate (toluene) liquid mixture is heated to 70 DEG C reaction (4 - 5) H test, free TDI 0.2%, adding 50% phenol (toluene) 15min reaction liquid is heated to 80 DEG C, and then heated to 90 DEG C, distilled acetone 1/2 dosage, 70 DEG C for standby. In ano

34、ther reactor with rapid stirring, adding two ethanol, three N- toluene ethylamine, ethylenediamine, deionized water on rapid mixing, the thermal insulation material at 70 DEG C, slowly added to the reactor, at 60 DEG C for neutralization reaction after transparent, is heated to 70 DEG C, vacuum pump

35、ing decompression distillation all the rest of the acetone, cooled to 40 DEG C, filtering and discharging.8 、 waterborne soybean oil acid polyester polyurethaneThe product formula (group A): OH: NCO (molar ratio) =1:1.5 resin, K = 1.019, R= 1.3, R =1.5 in excess of alcohol, oil 56%.Process steps: ac

36、cording to the formula will be soybean oil fatty acid, castor oil fatty acid, pentaerythritol, neopentyl glycol is added into the reaction kettle, pass into the CO 2 gas is heated to 120 DEG C to two lauric acid two butyl tin stirring, heating to 220 Deg. C, 3h reaction, cooling to 180 DEG C to benz

37、ene two formic acid, Benzene Partial anhydride and DMPA reaction at a temperature below 180 DEG 2h, every 30min sampling test until it reached 75mg KOH/g, acid value, hydroxyl value was 80, down to 120 deg.c toluene, heated to 132 DEG C reflux dehydration, Tuojin after cooling to 65 DEG C to 10% phe

38、nol toluene liquid mix, add TDI drops of monomer with the kettle, dropping, 1.5h drops after heating to 70 DEG C 4h, 80 degrees LH, test of free TDI in 0.2%, adding 50% phenol (toluene) liquid mix is heated to 90 DEG C for 15min reaction, vacuum extracting 2/3 toluene, adding isobutanol to cool 50 D

39、EG C, deionized water into three triethylamine, xylene ethanol amine and 1/3, adjusting the pH value of 8.6, up to 60 DEG C to transparent, vacuum pumping out all remaining toluene, deionized water, solid content 50%, adjust the filter material.9 、 waterborne vegetable oil alkyd polyurethaneThe prod

40、uct formula (group A): OH: NCO (molar ratio) =1:1.5, resin K =1.01, alcohol excess R= 1.314, r= 1.499, oil = 55.2%,Theoretical NCO content = 228%.Process steps: according to the formula (salad) rapeseed oil, castor oil fatty acid, TMP, neopentyl glycol is added into the reaction kettle, the CO2 gas

41、is heated to 120 DEG C with lithium naphthenate stirring, heating to 230 Deg. C reaction (2 3) H test, after passing the alcoholysis transparent cooling to 180 DEG C, adding two benzene anhydride, benzene anhydride, partial DMPA at 180 DEG C after reaction of 2h, every 30min, a test of acid value, u

42、ntil it reached 70mg KOH/ g, and then cooled to 110 DEG C with toluene, heated to 132 DEG C after dehydration, water removal, cooling to 65 DEG C with 10% phosphoric acid (a liquid benzene) mix, add TDI monomer dripping kettle, dropping, dropping after the reaction is heated to 70 DEG C (4 - 5) h, 8

43、0 degrees 1H, free TDI test reached 0.2%, adding 50% phenol (toluene) liquid is heated to 90 DEG C 15min, vacuum extrusion 1/3 adding toluene, isopropyl alcohol, drop Temperature to 50 deg.c N - two methyl diethanolamine, three ethylamine, deionized water and 1/2, adjusting the p value of H was 8.6, the reaction temperature is raised to 60 DEG C to transparent,