A kind of paste molecular sieve activation powder
Technical field
The present invention relates to a kind of molecular sieve preparation field technology, particularly a kind of paste molecular sieve activation powder.
Background technology
Reactive dual-component coating is present one type of more common coating, is divided into curing agent component and host component usually.The kind of this type coating is a lot, and range of application is also very wide, has favorable mechanical performance, higher solids content, is one type of rising coating variety at present.Modal reactive dual-component coating is a bicomponent polyurethane coating; Generally be made up of isocyanate prepolymer and hydroxy-containing resin two parts, main application direction has woodwork coating, car repair coating, anticorrosive paint, terrace lacquer, electronic paint, sapecial coating, polyurethane water-proof paint etc.
A lot of reactive dual-component coatings can react with the micro-moisture in system or the environment, finally cause in cured film, forming bubble, pin hole, also possibly reduce coating gloss.Therefore the moisture of removing in the reactive dual-component coating system is most important to its application.In the reactive dual-component coating there be the moisture source of trace: the micro-moisture that contains in the raw material, the water of pigment and filling surface absorption trace, the adsorbed water of coating in storage process, the moisture in construction environment.For eliminating the influence of micro-moisture, generally need in reactive dual-component coating, add deicer and remove moisture construction quality.The physics deicer is mainly molecular sieve, can remove the micro-moisture in the coating through in reactive dual-component coating, adding an amount of molecular sieve activation powder, guarantees construction quality, and molecular sieve activation powder can also play the strengthening action to coating simultaneously.
Be that mealy molecular sieve activation powder is directly added in the coating in early days, disperse inhomogeneously that complicated operation and part activation powder powder can fly away in air, cause wastage of material and very high dust pollution is arranged, working environment is more abominable; For head it off, my company proposes to make it to be in flow regime-paste through organic grease fixed member sieve activation powder, replaces mealy molecular sieve activation powder with paste molecular sieve activation powder, adding technology simply, be uniformly dispersed and do not influence working environment.
Organic dispersion medium must be avoided following problem with mixing of molecular sieve activation powder:
Molecular sieve activation powder is handled through high temperature dehydration; Water content is below 1.5%, and the moisture that in the preparation process, must control environment is when exposing in the air because of the activation powder; Micro-moisture is adsorbed by molecular sieve activation powder fast in the air; In 20min, adsorption moisture reaches more than 5%, has damaged the absorbent drying ability of molecular sieve.The preparation process adopts inert gas shielding among the present invention, stops the activation powder and directly contacts with air.
Molecular sieve activation powder mixes with organic dispersion medium for a long time; Moisture in the organic dispersion medium can be by molecular sieve adsorption; Cause adsorption capacity to descend, so organic dispersion medium must pass through deep dehydration, dehydration back organic media water content is reduced to below 0.001%.Can not influence the water separation capability of molecular sieve like this to polyurethane coating.
Effective mixing the between molecular sieve and the organic grease, must avoid organic grease to stop up molecular sieve pore passage, cause the part hole to stop up, do not have the effect of adsorption moisture.
Molecular sieve is a solid constituent, and bulk density is 0.7 g/ml more, and the low silica-alumina ratio molecular sieve is the high-hydrophilic material; And organic grease is hydrophobic grease, and lamination can appear in both mixing, through adding hydrophilic and oleophilic character in the viscosity modifier adjustment system; Through selecting effective viscosity modifier, and the ratio that adds solves the lamination problem that mixes, and makes molecular sieve abundant with mixing of organic dispersing agent; Bubble do not occur and pin hole is not reunited, place layering does not take place.
The paste molecular sieve activation powder of the present invention's preparation, the Static Water adsorbance has solved operating process to the ruined difficult problem of molecular sieve activation powder adsorption capacity more than 12% when 50% organic dispersing agent addition; Lotion after evenly disperseing is not stratified, wall built-up not; Solved bubble and wall cling phenomenon when the molecular sieve powder is applied to fluid-coating with paint, added organic dispersing agent molecular sieve activation powder afterwards, because the protective effect of organic dispersing agent; Make molecular sieve activation powder; Short time exposes in the air, can not absorb water fast and goes bad, and has reduced the operation easier that is applied in coating and the grease.
Summary of the invention
Technical problem to be solved by this invention provides a kind of paste molecular sieve activation powder, relates to a kind of dedicated molecular sieve used activation dried bean noodles of adsorption dewatering drying prescription that is used for fluent materials such as polyurethanes coating, paint.
For the purpose that realizes solving the problems of the technologies described above, the present invention has adopted following technical scheme:
A kind of paste molecular sieve activation powder of the present invention is characterised in that: paste molecular sieve activation powder is to become molecular screen primary powder 48%-52%, the castor oil 30%-52% of high-temperature roasting dehydration, the mixer kneader thing of viscosity modifier 0%-20% by quality group; Described viscosity modifier is the mixture of any or arbitrary proportion of o-phthalic acid dibutyl ester (DOP), propane diols, butanediol, diglycol, triethylene-glycol, PEG400 (PEG-400), Macrogol 600 (PEG-600), polypropylene glycol 400 (PPG-400), polypropylene glycol 600 (PPG-600), polypropylene glycol 1000 (PPG-1000), polypropylene glycol 2000 (PPG-2000).Described molecular screen primary powder comprises 3A, 4A, 13X etc.Preferred molecular screen primary powder Static Water is adsorbed as between the 26.5%-34%.Preferred molecular sieve is 3A, 4A molecular screen primary powder, and Static Water is adsorbed as between the 26.5%-28%.
The preparation method of a kind of paste molecular sieve activation powder of the present invention comprises following flow process, i.e. molecular sieve calcination activation, batching, mixer kneader, roll; Detailed process is:
(1), calcination activation
Molecular screen primary powder is keeping under the complete situation of molecular sieve structure it through 400 ℃ of-750 ℃ of high-temperature roastings dehydration activation, and residual moisture content is controlled at below 1.5%; Described molecular screen primary powder comprises 3A, 4A, 13X etc.The Static Water of preferred molecular screen primary powder is adsorbed as between the 26.5%-34%.Preferred molecular screen primary powder is 3A, 4A molecular screen primary powder, and Static Water is adsorbed as between the 26.5%-28%.
Residual moisture content is preferably in below 0.5%, to guarantee molecular screen primary powder normal temperature adsorption capacity.
The purpose of roasting is roasting dehydration activation, makes it have very strong water absorption ability, through keeping the complete and height activation of molecular sieve structure.
Sample is different according to the different adsorption capacities of kind after the activation, generally between 25-33%.
(2), batching
With the former powder of mealy molecular sieve, castor oil and viscosity modifier by weight, the ratio of the former powder 48%-52% of mealy molecular sieve, castor oil 30%-52%, viscosity modifier 0%-20% is prepared burden.
Wherein the castor oil of selecting for use comprises dehydrated castor oil, rilanit special, sulfonated castor oil, ricinoleate ester etc., and two or more mixture wherein.
Institute's castor oil of selecting for use is all through the dehydration preliminary treatment.Concrete processing method is: add 0.5% hydroquinones in the castor oil, be heated to 120 ℃, vacuumize dehydration 2h.
Described viscosity modifier is: the mixture of any of o-phthalic acid dibutyl ester (DOP), propane diols, butanediol, diglycol, triethylene-glycol, PEG400 (PEG-400), Macrogol 600 (PEG-600), polypropylene glycol 400 (PPG-400), polypropylene glycol 600 (PPG-600), polypropylene glycol 1000 (PPG-1000), polypropylene glycol 2000 (PPG-2000) or arbitrary proportion.
(3), mixer kneader
The former powder of castor oil, viscosity modifier and mealy molecular sieve is added mixer kneader in the kneader, and kneader is through vacuumizing processing, or charges into inert gas; Wherein castor oil and viscosity modifier are through heat treated, and temperature is controlled between 20 ℃-100 ℃, preferred 20 ℃-70 ℃; Incorporation time does not wait according to the different 0.5h-5h of proportioning, preferred 1h-2h.Inert gas comprises nitrogen, argon gas etc.Application of vacuum or charge into inert gas in order to get rid of to mediate the moisture in the environment avoids operating process to lose efficacy because of the molecular sieve suction.
(4), roll
Transfer in the multistage roller mill mediating afterproduct in the kneader, mixing 10min-100min under 10 ℃-100 ℃; Operate in air, inert protective gas or vacuumize under the state; With the product that mixes pack into container, sealing, promptly get product at last.
Temperature can be preferred 20 ℃-70 ℃; Incorporation time is according to the preferred 20-30min of proportioning; Operation is preferably carried out under vacuum state.
The application of a kind of paste molecular sieve activation powder of the present invention aspect adsorption dewatering; Characteristic is that paste molecular sieve activation powder is applied to Central Plains, field material dehydration such as polyurethane coating, paint; Keep properties of product; It is bad to prevent that coating from use disperseing, and causes foaming, wall built-up, mobile difference phenomenon.
The described ion-exchange degree of this patent if no special instructions, is the molar percentage exchange degree.Described other compositions of this patent, water content and mixed proportion if no special instructions, are the mass percent example for solid and liquid, are percent by volume for gas.
These technical schemes also can mutual combination perhaps combine, thereby reach better technique effect.
Through adopting technique scheme, the present invention has following beneficial effect:
The paste molecular sieve activation powder of the present invention's preparation keeps the water adsorption capacity of activation powder not destroy, and the lotion water adsorption amount that obtains is more than 12%; Avoid reuniting and bubble, product is not stratified, wall built-up not, easy to use and operation; Organic dispersion medium protection powder, the short time exposes in the air can not destroy the water adsorption capacity.
The specific embodiment
Below in conjunction with embodiment this patent is further explained.But the protection domain of this patent is not limited to concrete embodiment.
Molecular screen primary powder among the embodiment is the molecular screen primary powder of the preparation of known technology, and other is chemical pure or industrial raw material unless stated otherwise, and water absorption test is 25 ℃, tests under 50% relative humidity.Institute's castor oil of selecting for use is all through the dehydration preliminary treatment.The concrete processing method of castor oil dehydration preliminary treatment is: add 0.5% hydroquinones in the castor oil, be heated to 120 ℃, vacuumize dehydration 2h.
Step that embodiment adopted and method roughly the same specify in embodiment 1, except that necessary person, all only sketch its principal character.
Embodiment 1
3A molecular sieve activation powder JLH-03B (exchange degree the is 45%) 52g of castor oil 48g and Luoyang Jianlong Chemical Industry Co., Ltd.'s production to be added in the vacuum kneader, under 70 ℃ of conditions, mediate 2h, in order to mix better more equably; Prevent caking etc.; To mediate machine mixing afterproduct and transfer in the multistage roller mill, mixing 30min under 70 ℃ of conditions, product mixes; Wall built-up does not have the viscosity of higher flowability and suitable operation.Normal temperature test absorption property 12h water adsorption amount is 5.4%, and the absorption of 24h water reaches 7.8%, and water absorption reaches capacity 12.5% basically after greater than 72h, and along with the increase of adsorption time, adsorbance no longer increases.This sample has the moderate rate of adsorption, can not expose air and absorbs water strongly and lost efficacy because of the short time, and is therefore stronger to the adaptive capacity of environment, is convenient in varying environment, operate.
Embodiment 2
Repeat embodiment 1, difference is castor oil 52g and molecular sieve activation powder JLH-03B 48g are added in the vacuum kneader, under 60 ℃ of conditions, mediates 1h, and product is transferred in the multistage roller mill afterwards, mixing 20min under 60 ℃ of conditions.Normal temperature test absorption property 12h water adsorption amount is 5.6%, and the absorption of 24h water reaches 7.6%, and water absorption reaches capacity 12.1% basically after greater than 72h.
Embodiment 3
Repeat embodiment 1; Difference is castor oil 30g, o-phthalic acid dibutyl ester (DOP) 20g and molecular sieve activation powder JLH-03B 50g are added in the vacuum kneader; Under 20 ℃ of conditions, mediate 1h, product is transferred in the multistage roller mill afterwards, mixing 10min under 20 ℃ of conditions.Normal temperature test absorption property 12h water adsorption amount is 6.7%, and the absorption of 24h water reaches 9.7%, and water absorption reaches capacity 12.3% basically after greater than 72h.
Embodiment 4:
Repeat embodiment 1; Difference is castor oil 37g, o-phthalic acid dibutyl ester (DOP) 13g and molecular sieve activation powder JLH-03B 50g are added in the vacuum kneader; Under 30 ℃ of conditions, mediate 1h, product is transferred in the multistage roller mill afterwards, mixing 20min under 30 ℃ of conditions.Normal temperature test absorption property 12h water adsorption amount is 6.3%, and the absorption of 24h water reaches 8.7%, and water absorption reaches capacity 12.7% basically after greater than 72h.
Embodiment 5:
Repeat embodiment 1, difference is castor oil 42g, propane diols 8g and molecular sieve activation powder JLH-03B 50g are added in the vacuum kneader, under 30 ℃ of conditions, mediates 1.5h, and product is transferred in the multistage roller mill afterwards, mixing 20min under 30 ℃ of conditions.Normal temperature test absorption property 12h water adsorption amount is 6.7%, and the absorption of 24h water reaches 8.8%, and water absorption reaches capacity 12.4% basically after greater than 72h.
Embodiment 6:
Repeat embodiment 1, difference is castor oil 40g, butanediol 10g and molecular sieve activation powder JLH-03B50g are added in the vacuum kneader, under 40 ℃ of conditions, mediates 1h, and product is transferred in the multistage roller mill afterwards, mixing 20min under 40 ℃ of conditions.Normal temperature test absorption property 12h water adsorption amount is 6.0%, and the absorption of 24h water reaches 8.9%, and water absorption reaches capacity 12.9% basically after greater than 72h.
Embodiment 7:
Repeat embodiment 1; Difference is castor oil 38g, diglycol 12g and molecular sieve activation powder JLH-03B50g are added in the vacuum kneader; Under 40 ℃ of conditions, mediate 1h, product is transferred in the multistage roller mill afterwards, mixing 20min under 40 ℃ of conditions.Normal temperature test absorption property 12h water adsorption amount is 6.8%, and the absorption of 24h water reaches 8.4%, and water absorption reaches capacity 12.7% basically after greater than 72h.
Embodiment 8:
Repeat embodiment 1; Difference is castor oil 36g, triethylene-glycol 14g and molecular sieve activation powder JLH-03B50g are added in the vacuum kneader; Under 40 ℃ of conditions, mediate 1h, product is transferred in the multistage roller mill afterwards, mixing 20min under 40 ℃ of conditions.Normal temperature test absorption property 12h water adsorption amount is 6.5%, and the absorption of 24h water reaches 8.7%, and water absorption reaches capacity 12.4% basically after greater than 72h.
Embodiment 9:
Repeat embodiment 1; Difference is castor oil 40g, PEG400 (PEG-400) 10g and molecular sieve activation powder JLH-03B50g are added in the vacuum kneader; Under 30 ℃ of conditions, mediate 1h, product is transferred in the multistage roller mill afterwards, mixing 20min under 30 ℃ of conditions.Normal temperature test absorption property 12h water adsorption amount is 6.7%, and the absorption of 24h water reaches 8.9%, and water absorption reaches capacity 12.5% basically after greater than 72h.
Embodiment 10:
Repeat embodiment 1; Difference is castor oil 38g, Macrogol 600 (PEG-600) 12g and molecular sieve activation powder JLH-03B50g are added in the vacuum kneader; Under 50 ℃ of conditions, mediate 1h, product is transferred in the multistage roller mill afterwards, mixing 10min under 50 ℃ of conditions.Normal temperature test absorption property 12h water adsorption amount is 6.3%, and the absorption of 24h water reaches 8.2%, and water absorption reaches capacity 12.1% basically after greater than 72h.
Embodiment 11:
Repeat embodiment 1; Difference is castor oil 42g, polypropylene glycol 400 (PPG-400) 8g and molecular sieve activation powder JLH-03B50g are added in the vacuum kneader; Under 30 ℃ of conditions, mediate 1h, product is transferred in the multistage roller mill afterwards, mixing 20min under 30 ℃ of conditions.Normal temperature test absorption property 12h water adsorption amount is 6.2%, and the absorption of 24h water reaches 8.4%, and water absorption reaches capacity 12.3% basically after greater than 72h.
Embodiment 12:
Repeat embodiment 1; Difference is castor oil 39g, polypropylene glycol 600 (PPG-600) 11g and molecular sieve activation powder JLH-03B 50g are added in the vacuum kneader; Under 40 ℃ of conditions, mediate 1h, product is transferred in the multistage roller mill afterwards, mixing 20min under 40 ℃ of conditions.Normal temperature test absorption property 12h water adsorption amount is 6.4%, and the absorption of 24h water reaches 8.7%, and water absorption reaches capacity 12.2% basically after greater than 72h.
Embodiment 13:
Repeat embodiment 1; Difference is castor oil 37g, polypropylene glycol 1000 (PPG-1000) 13g and molecular sieve activation powder JLH-03B50g are added in the vacuum kneader; Under 30 ℃ of conditions, mediate 1h, product is transferred in the multistage roller mill afterwards, mixing 20min under 30 ℃ of conditions.Normal temperature test absorption property 12h water adsorption amount is 6.6%, and the absorption of 24h water reaches 8.2%, and water absorption reaches capacity 12.2% basically after greater than 72h.
Embodiment 14:
Repeat embodiment 1; Difference is castor oil 36g, polypropylene glycol 2000 (PPG-2000) 14g and molecular sieve activation powder JLH-03B 50g are added in the vacuum kneader; Under 40 ℃ of conditions, mediate 1h, product is transferred in the multistage roller mill afterwards, mixing 20min under 30 ℃ of conditions.Normal temperature test absorption property 12h water adsorption amount is 6.1%, and the absorption of 24h water reaches 8.4%, and water absorption reaches capacity 12.4% basically after greater than 72h.
Embodiment 15:
Repeat embodiment 1, difference is that molecular sieve activation powder is the 4A molecular sieve activation powder JLH-04 that Luoyang Jianlong Chemical Industry Co., Ltd. produces.Normal temperature test absorption property 12h water adsorption amount is 6.3%, and the absorption of 24h water reaches 9.2%, and water absorption reaches capacity 13.2% basically after greater than 72h.
Embodiment 16:
Repeat embodiment 1, difference is castor oil without processed, and normal temperature test absorption property 12h water adsorption amount is 3.4%, and the absorption of 24h water reaches 5.6%, and water absorption reaches capacity 6.2% basically after greater than 72h.