CN112058218A - Preparation method of professional molecular sieve drying agent for brake system - Google Patents
Preparation method of professional molecular sieve drying agent for brake system Download PDFInfo
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- 239000002808 molecular sieve Substances 0.000 title claims abstract description 93
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 title claims abstract description 93
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000002274 desiccant Substances 0.000 title claims abstract description 19
- 238000005096 rolling process Methods 0.000 claims abstract description 93
- 229910021536 Zeolite Inorganic materials 0.000 claims abstract description 68
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims abstract description 68
- 239000010457 zeolite Substances 0.000 claims abstract description 68
- 239000000843 powder Substances 0.000 claims abstract description 45
- 238000002156 mixing Methods 0.000 claims abstract description 44
- 239000000853 adhesive Substances 0.000 claims abstract description 43
- 230000001070 adhesive effect Effects 0.000 claims abstract description 43
- 238000001035 drying Methods 0.000 claims abstract description 41
- 239000002994 raw material Substances 0.000 claims abstract description 29
- 238000012216 screening Methods 0.000 claims abstract description 27
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 21
- 239000010703 silicon Substances 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 19
- 239000002904 solvent Substances 0.000 claims abstract description 14
- 238000007873 sieving Methods 0.000 claims abstract description 13
- 230000017525 heat dissipation Effects 0.000 claims abstract description 5
- 238000009461 vacuum packaging Methods 0.000 claims abstract description 3
- 238000009489 vacuum treatment Methods 0.000 claims abstract description 3
- 230000007246 mechanism Effects 0.000 claims description 101
- 230000006835 compression Effects 0.000 claims description 83
- 238000007906 compression Methods 0.000 claims description 83
- 239000000463 material Substances 0.000 claims description 73
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 54
- 238000005507 spraying Methods 0.000 claims description 53
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 44
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 42
- 239000007921 spray Substances 0.000 claims description 31
- 239000005995 Aluminium silicate Substances 0.000 claims description 24
- 235000012211 aluminium silicate Nutrition 0.000 claims description 24
- 239000000203 mixture Substances 0.000 claims description 24
- 238000000227 grinding Methods 0.000 claims description 21
- 238000000498 ball milling Methods 0.000 claims description 19
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 13
- 239000011344 liquid material Substances 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 10
- 229960000892 attapulgite Drugs 0.000 claims description 9
- 239000000440 bentonite Substances 0.000 claims description 9
- 229910000278 bentonite Inorganic materials 0.000 claims description 9
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 9
- 229910052625 palygorskite Inorganic materials 0.000 claims description 9
- 238000007599 discharging Methods 0.000 claims description 8
- 239000008187 granular material Substances 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 239000011230 binding agent Substances 0.000 claims description 7
- 238000003860 storage Methods 0.000 claims description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 6
- 229910052681 coesite Inorganic materials 0.000 claims description 6
- 229910052593 corundum Inorganic materials 0.000 claims description 6
- 229910052906 cristobalite Inorganic materials 0.000 claims description 6
- 238000002425 crystallisation Methods 0.000 claims description 6
- 230000008025 crystallization Effects 0.000 claims description 6
- 239000000377 silicon dioxide Substances 0.000 claims description 6
- 235000012239 silicon dioxide Nutrition 0.000 claims description 6
- 229910052682 stishovite Inorganic materials 0.000 claims description 6
- 229910052905 tridymite Inorganic materials 0.000 claims description 6
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 6
- 230000032683 aging Effects 0.000 claims description 5
- 238000001879 gelation Methods 0.000 claims description 5
- 238000001802 infusion Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 241001494479 Pecora Species 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 4
- 208000005156 Dehydration Diseases 0.000 claims description 3
- 235000013421 Kaempferia galanga Nutrition 0.000 claims description 3
- 244000062241 Kaempferia galanga Species 0.000 claims description 3
- 230000018044 dehydration Effects 0.000 claims description 3
- 238000006297 dehydration reaction Methods 0.000 claims description 3
- 238000000967 suction filtration Methods 0.000 claims description 3
- 230000008878 coupling Effects 0.000 claims description 2
- 238000010168 coupling process Methods 0.000 claims description 2
- 238000005859 coupling reaction Methods 0.000 claims description 2
- 238000001179 sorption measurement Methods 0.000 abstract description 19
- 238000005299 abrasion Methods 0.000 abstract description 14
- 238000012360 testing method Methods 0.000 description 32
- 239000000523 sample Substances 0.000 description 25
- 230000003068 static effect Effects 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 9
- 239000012798 spherical particle Substances 0.000 description 9
- 229910052573 porcelain Inorganic materials 0.000 description 7
- 238000010586 diagram Methods 0.000 description 5
- 239000011148 porous material Substances 0.000 description 5
- 241000283707 Capra Species 0.000 description 4
- 235000009508 confectionery Nutrition 0.000 description 4
- 239000011265 semifinished product Substances 0.000 description 4
- 238000004891 communication Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000014759 maintenance of location Effects 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000010981 drying operation Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 241001391944 Commicarpus scandens Species 0.000 description 1
- MXRIRQGCELJRSN-UHFFFAOYSA-N O.O.O.[Al] Chemical compound O.O.O.[Al] MXRIRQGCELJRSN-UHFFFAOYSA-N 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- CQBLUJRVOKGWCF-UHFFFAOYSA-N [O].[AlH3] Chemical compound [O].[AlH3] CQBLUJRVOKGWCF-UHFFFAOYSA-N 0.000 description 1
- OBNDGIHQAIXEAO-UHFFFAOYSA-N [O].[Si] Chemical compound [O].[Si] OBNDGIHQAIXEAO-UHFFFAOYSA-N 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 239000013068 control sample Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 239000006069 physical mixture Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 239000011882 ultra-fine particle Substances 0.000 description 1
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/16—Alumino-silicates
- B01J20/18—Synthetic zeolitic molecular sieves
- B01J20/183—Physical conditioning without chemical treatment, e.g. drying, granulating, coating, irradiation
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- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The application belongs to the technical field of molecular sieves, and particularly relates to a preparation method of a professional molecular sieve drying agent of a brake system, which comprises the following steps: preparing synthetic zeolite raw powder; uniformly mixing raw materials: putting the synthetic zeolite and the adhesive into a premixing device according to the proportion and mixing; rolling ball treatment, namely vibrating and screening, performing secondary rolling ball operation, and adding 2-6 wt% of inorganic silicon solvent in the secondary rolling ball process; drying, wherein the humidity of the molecular sieve is controlled to be 20-40% of the total weight of the molecular sieve; roasting: the dried molecular sieve is sent into a roasting furnace and roasted for 30 to 120 minutes at the temperature of 200-850 ℃; screening and heat dissipation: sieving and radiating the roasted molecular sieve; and (4) performing vacuum treatment, packaging and warehousing. The method adopts the synthetic zeolite raw powder as the raw material, not only has lower cost, but also has uniform size and quality of the finished molecular sieve, and has better adsorption capacity and lower abrasion rate.
Description
Technical Field
The application relates to the technical field of molecular sieve production, in particular to a preparation method of a professional molecular sieve drying agent of a brake system.
Background
Molecular sieves are crystalline silicates or aluminosilicates formed from silicon-oxygen tetrahedra or aluminum-oxygen tetrahedra connected by oxygen bridges. The molecular sieve has a uniform microporous structure, the diameter of the pores is uniform, the pores can adsorb molecules smaller than the diameter of the pores into the pores and have preferential adsorption capacity on polar molecules and unsaturated molecules, so that the molecular sieve can separate the molecules with different polarity degrees, different saturation degrees of increased bonds, different molecular sizes and different boiling points, namely has the function of sieving the molecules, and is called as the molecular sieve. At present, the molecular sieve has the advantages of high adsorption capacity, strong thermal stability and the like which are not possessed by other adsorbents, so that the molecular sieve can be widely applied to the fields of automobiles, building glass, medicines, paints and the like.
The molecular sieve special for commercial vehicles, which is arranged in an air brake system of the vehicle, has the advantages of drying gas in the brake system to control moisture in the brake system and prevent brake slip, and the prior Chinese invention patent application with the publication number of CN1082000A discloses a method for producing the molecular sieve by using a natural zeolite raw material, wherein the molecular sieve adopts the natural zeolite as the raw material, and the specific operation is as follows: baking the selected raw materials at 90-200 ℃ for 1-6 hours, grinding the raw materials to 85-500 meshes, roasting the raw materials at 500-1000 ℃ for 2-6 hours to destroy the crystal structure of the raw materials, adding a certain amount of hydroxide (the weight ratio of the raw materials to the hydroxide is (2-4): 1), fully stirring, and uniformly mixing to obtain a semi-finished product. And (3) aging the semi-finished product at 40-100 ℃ for 2-4 hours, heating to 100-200 ℃, crystallizing for 2-8 hours, stirring, filtering, washing and drying to obtain the 4A type zeolite molecular sieve raw powder.
Then 10 kg of raw materials are baked for 4 hours at 90 ℃, ground to 100 meshes, baked for 3 hours at 800 ℃, added with 2kg of sodium hydroxide and fully stirred, and evenly mixed to obtain a semi-finished product. Aging the semi-finished product at 60 ℃ for 3 hours, heating to 150 ℃ for crystallization for 7 hours, stirring, filtering, washing, drying, adding a sodium silicate adhesive and a small amount of water into the obtained zeolite raw powder according to the proportion of 20 percent of the total weight, uniformly mixing, and balling to obtain the 4A type natural zeolite molecular sieve.
The above prior art solutions have the following drawbacks: the molecular sieve adopts natural zeolite as a raw material, firstly, the natural zeolite has limited resources, high cost and low yield, and the particle size and the shape of the natural zeolite are different, so that the finally prepared molecular sieve has larger difference of the size and the mass of a formed particle, and a new technical scheme is required to solve the problems.
Disclosure of Invention
Aiming at the defects in the prior art, one of the purposes of the invention is to provide a preparation method of a professional molecular sieve desiccant for a brake system, and the method adopts synthetic zeolite raw powder as a raw material, so that the cost is lower, the size and the quality of a finished molecular sieve are uniform, and the molecular sieve has better adsorption capacity and abrasion rate.
The above application purpose of the present application is achieved by the following technical solutions: a preparation method of a professional molecular sieve desiccant for a brake system comprises the following steps:
step one, preparing synthetic zeolite raw powder;
step two, uniformly mixing the raw materials: mixing the synthetic zeolite and the binder in the first step according to the mass ratio of (60-80): (2-4) putting into a premixing device for mixing;
step three, rolling ball treatment: putting the material in the step two into a ball rolling device for ball rolling treatment, wherein the rotating speed of the ball rolling device is 30-120 r/min;
step four, vibration screening, carrying out secondary rolling operation, and adding 2-6 wt% of inorganic silicon solvent in the secondary rolling process;
step five, drying: drying the material obtained by screening in the step 4 at the temperature of 60-120 ℃, and controlling the humidity of the dried molecular sieve to be 20-40% of the total weight of the molecular sieve;
step six, roasting: feeding the dried molecular sieve in the step five into a roasting furnace, and roasting at the temperature of 200-850 ℃ for 30-120 minutes;
step seven, screening and heat dissipation: screening and radiating the material obtained by roasting in the step six;
and step eight, carrying out vacuum treatment, packaging and warehousing.
By adopting the technical scheme, the synthetic zeolite raw powder which is automatically synthesized is adopted as a raw material to replace natural zeolite as a raw material, so that the preparation cost can be reduced, the size and the quality uniformity of the finished molecular sieve can be ensured, the synthetic zeolite and the adhesive are mixed in a pre-mixing device which is automatically designed according to the mass ratio, the dispersion effect of the synthetic zeolite and the adhesive can be ensured, the treatment efficiency of the ball rolling treatment in the next step is facilitated, and the quality of ball forming is ensured; in the rolling ball treatment, a self-improved rolling ball device is adopted for treatment, so that the uniformity of the grain diameter of the rolling balls and the rolling ball treatment efficiency can be ensured, the inorganic silicon solvent can be uniformly distributed on the surfaces of the rolling balls, and the step six of roasting and sintering to form the 4A spherical molecular sieve is facilitated; in the drying step, the moisture in the molecular sieve is emitted to the surface of the molecular sieve, and the moisture on the surface of the molecular sieve can be emitted, so that the water content in the molecular sieve is reduced, and the phenomenon of sticky particles is avoided; controlling the humidity of the dried molecular sieve to be 20-40% of the total weight of the molecular sieve, uniformly distributing water in the molecular sieve and on the surface of the molecular sieve, roasting the molecular sieve in a roasting furnace, and sintering the roasted molecular sieve into spheres at high temperature.
Preferably, in the step one, the preparation of the synthetic zeolite raw powder specifically comprises: step 1.1, raw material pretreatment: selecting kaolin with the SiO2/Al2O3 molar ratio of 2.15-2.20, grinding, and sieving with a 600-1340 mesh sieve;
step 1.2, dehydration treatment: roasting and dehydrating the kaolin obtained by screening at the temperature of 650-850 ℃ to obtain metakaolin;
step 1.3, screening: sieving with a 1000-1340 mesh sieve;
step 1.4, gelation: preparing a sodium hydroxide solution with the concentration of 2.45-3.65 mol/L, wherein the mass ratio of the amount of the metakaolin to the sodium hydroxide solution in the step 1.3 is 1: (45-60), adding the metakaolin obtained in the step 1.2 into a sodium hydroxide solution, and stirring and gelling at the temperature of 60-80 ℃;
step 1.5, aging treatment: transferring the material obtained in the step 1.4 to an environment with the temperature of 18-25 ℃, and standing for 1-2 hours;
step 1.6, crystallization treatment: transferring the material obtained in the step 1.5 to an environment with the temperature of 60 +/-3 ℃, heating to 90 +/-1.0 ℃ at the heating speed of 2.5 +/-0.3 ℃, and preserving heat for 2-4 hours;
and step 1.7, carrying out suction filtration and washing until the pH value is 10-12, and drying at 100 ℃ to obtain the 4A molecular sieve raw powder.
The 4A molecular sieve raw powder prepared by the method has the crystallization rate of 94.5-95.2%, the SiO2/Al2O3 molar ratio of 2.05-2.15 is selected to ensure the utilization rate of the raw materials, and the kaolin is crushed and sieved to obtain fine-particle kaolin with the particle size of 10-23 mu m, so that the high-quality metakaolin is conveniently obtained by roasting and dehydrating; the metakaolin is obtained by roasting and dehydrating at the temperature of 650-850 ℃, and is a physical mixture of amorphous alumina and amorphous silica, and the state ensures that the metakaolin has high chemical reaction activity and is beneficial to converting silicon and aluminum into a 4A molecular sieve; screening to obtain metakaolin with the particle size of 10-13 mu m, carrying out sodium hydroxide solution treatment, stirring and condensing to form colloid, standing for 1-2 hours in an environment of 18-25 ℃ to age and form tiny crystal nuclei, and then carrying out crystallization treatment to obtain synthetic zeolite raw powder with uniform particle size and quality and good adsorption capacity and abrasion rate, so that the quality of the spherical 4A molecular sieve prepared by the synthetic zeolite raw powder can be ensured.
Preferably, the adhesive in the step 1 comprises 40-60% of kaolin, 10-25% of attapulgite, 10-25% of sheep's-sweet soil and 5-10% of bentonite by mass percent.
The adhesive takes kaolin as a main material and is supplemented with attapulgite, goat's sweet earth and bentonite, so that the treatment efficiency of rolling balls is effectively ensured, the synthetic zeolite raw powder and the adhesive can be quickly bonded into balls, the binding power between the synthetic zeolite raw powder is ensured, and the later-stage drying roasting treatment is facilitated; the humidity of the spherical particles bonded by the adhesive is easily controlled to be 28-33% during drying, so that the quality of the molecular sieve dried in the step five is ensured, and the particles are prevented from being bonded with each other.
Preferably, the premixing device comprises a bracket with a three-layer structure, a premixing mechanism, a compression mechanism, a crushing mechanism and a ball milling mechanism, wherein the bracket is sequentially provided with a first mounting layer, a second mounting layer and a third mounting layer from bottom to top; the premixing mechanism is arranged on the third mounting layer and communicated with the compression mechanism; the compression mechanism is arranged on the second mounting layer and is communicated with the breaking mechanism; the smashing mechanism is communicated with the first mounting layer and can be communicated with the ball milling mechanism; the ball milling mechanism is arranged on the ground.
The synthetic zeolite raw powder and the adhesive are fully dispersed by adopting a premixing mechanism, the powder mixed and dispersed by the premixing mechanism is compressed into blocks by a compression mechanism, then the materials compressed into blocks are crushed and ground by a crushing mechanism to obtain a high-dispersity synthetic zeolite raw powder and adhesive mixture, and finally the high-dispersity synthetic zeolite raw powder and adhesive mixture is subjected to ball milling treatment by a ball milling mechanism to obtain the superfine and high-dispersity synthetic zeolite raw powder and adhesive mixture, so that the subsequent ball rolling treatment is facilitated to obtain the quality of spherical particles, the subsequent drying and roasting treatment operations are also facilitated to be carried out, and the 4A spherical molecular sieve with higher adsorption capacity, better stacking density and better abrasion rate is obtained.
Preferably, the premixing mechanism comprises a mixing tank and a screw conveying assembly, wherein the screw conveying assembly is arranged in the mixing tank and is used for mixing the synthetic zeolite and the adhesive; one end of the mixing tank body is circumferentially communicated with a feeding pipe; the end of the feeding pipe is connected with a sealing cover through threads; the other end of the mixing tank body is circumferentially communicated with a discharge pipe; the discharge pipe is communicated with the compression mechanism; the discharge pipe is provided with an electromagnetic valve; the electromagnetic valve is positioned in the circumferential direction of the mixing tank body; the spiral conveying assembly comprises a double-spiral stirrer rotatably connected in the mixing tank body and a servo motor driving the double-spiral stirrer to rotate, and the central axis of the double-spiral stirrer is superposed with the central axis of the mixing tank body; the pipe end of the double-helix stirrer, which is positioned at the outer side of the mixing tank body, is fixedly connected with an output shaft of the servo motor through a coupler; the servo motor is fixedly connected to the third mounting layer through bolts; the compression mechanism comprises a compression pipe, a first compression piece and a second compression piece, wherein the first compression piece and the second compression piece are respectively arranged at the pipe end of the compression pipe and are used for compressing the synthetic zeolite and the adhesive into blocks; the first compression piece and the second compression piece are identical in structure; the first compression piece comprises an air cylinder and a compression block, and the compression block is fixedly connected to a push rod of the air cylinder; the compression block can move along the axial direction of the compression pipe; the second mounting layer is provided with a channel for the compressed material to flow to the breaking mechanism; the discharging pipe is communicated with the periphery of the compression pipe.
The positive rotation and the negative rotation of the double-helix stirrer are controlled by a servo motor, and the double-helix stirrer is repeatedly used for many times, so that the synthetic zeolite and the adhesive can be fully mixed; the material mixed by the premixing mechanism flows into the compression pipe through the discharge pipe, the compression block of the first compression piece is kept still, the cylinder of the second compression piece is started, the compression block of the second compression piece is driven to move towards the compression block of the first compression piece, so that the mixed material is compressed into blocks, then the cylinder of the first compression piece is started, the compression block of the first compression piece moves leftwards, the cylinder of the second compression piece is started, the compression block of the second compression piece pushes the material compressed into blocks out of the compression pipe, the material flows into the crushing mechanism through the channel to be crushed, and the mixed material is pressed into blocks.
Preferably, the crushing mechanism comprises a shell, a pair of crushing rollers for crushing the compressed materials, a pair of grinding rollers for grinding the crushed materials and a collecting hopper for collecting the ground materials, wherein the connecting line of the planes of the central axes of the two crushing rollers is a horizontal plane; the connecting line of the planes of the central axes of the two grinding rollers is a horizontal plane; the connecting line of the tangent points of the two crushing rollers and the tangent points of the two crushing rollers is vertical to the surface of the first mounting layer; the vertical projections of the crushing roller and the rolling roller are both in the vertical projection of the collecting hopper; the bottom of the collecting hopper is funnel-shaped and is communicated with a discharging pipe fitting; the discharge pipe fitting comprises a straight pipe communicated with the bottom of the collecting hopper, a control valve arranged on the straight pipe and an extension pipe communicated with the straight pipe, and the extension pipe can add materials to be ball-milled to the ball-milling mechanism; the ball milling mechanism is a planetary ball mill.
The mixed materials are pressed into blocks, wherein the fineness of the granules is screened, the granules are similar in granularity, the granules are easy to break into small blocks under the action of a breaking roller, and the small blocks flow to a grinding roller to be ground and milled to obtain the synthetic zeolite raw powder and the adhesive mixture with uniform particle size and good dispersity; then the mixture is ball milled by a planetary ball mill to obtain the superfine and high-dispersion synthetic zeolite raw powder and the adhesive mixture.
Preferably, the ball rolling device comprises a ball rolling tank body, a driving mechanism for driving the ball rolling tank body to rotate around the axial direction of the ball rolling tank body, an adjusting mechanism and a liquid material spraying mechanism, wherein the adjusting mechanism is used for adjusting the inclination angle of the ball rolling tank body; the liquid material spraying mechanism is used for spraying liquid materials into the rolling ball tank body; the driving mechanism comprises a supporting body, a connecting column hinged to the middle part of the supporting body, a connecting rod, a driven gear, a motor and a driving gear, wherein one end of the connecting rod is welded at the center of the bottom of the spin tank body, and the other end of the connecting rod is rotatably connected to the connecting column; the driven gear is fixedly connected to the circumferential direction of the connecting rod and meshed with the driving gear; the driving gear is fixedly connected to the circumferential direction of the output shaft of the motor; the motor is fixedly connected to the circumferential direction of the connecting column; the adjusting mechanism comprises a base and a cylinder; the base is fixedly connected to the ground; the cylinder is fixedly connected to the base; a push rod of the air cylinder is fixedly connected to the periphery of the column end of the connecting column, which is opposite to the rolling ball tank body; the liquid material spraying mechanism comprises a water tank, an inorganic silicon solvent storage tank, a centrifugal pump and a spraying assembly, wherein one end of the centrifugal pump is communicated with a first liquid conveying pipe, and the other end of the centrifugal pump is communicated with a second liquid conveying pipe; the water tank is communicated with a water delivery pipe; the water delivery pipe is communicated with the circumferential direction of the second liquid delivery pipe; the water delivery pipe is provided with a first ball valve; the inorganic silicon solvent storage tank is communicated with a conveying pipe; the conveying pipe is communicated with the circumferential direction of the second infusion pipe; the conveying pipe is provided with a second ball valve; the spraying assembly comprises a spraying main pipe and a spraying head, one end of the spraying main pipe is communicated with the first liquid conveying pipe in a threaded mode, the other end of the spraying main pipe is communicated with the spraying head, and a pulse valve is arranged on the spraying main pipe; the spray header comprises a hollow sphere, a plurality of spray pipes and a plurality of spray headers, and the hollow sphere is integrally formed with a cavity; the spray pipe is fixedly connected with the hollow sphere; one end of the spray pipe is communicated with the cavity; the spray header is communicated with the other end of the spray pipe; the spray head faces the interior of the rolling ball tank body; .
The water body and the inorganic silicon solvent can be conveniently sprayed to the materials in the rolling ball tank body through the spray head, and can be uniformly distributed on the surfaces of the spherical particles; the quality of the ball treatment is ensured.
Preferably, in step three, the rolling ball is operated in a specific manner as follows: and (3) adding the material obtained in the second step into the rolling ball device under the rotation of 60 revolutions per minute, spraying water on the outer surface of the material obtained in the second step, continuously rolling for 20-25 minutes at the rolling ball speed of 60-120 revolutions per minute, then spraying water again and spraying an adhesive, continuously rolling for 5-10 minutes, and repeating the following operations: spraying water on the outer surface of the material obtained in the step two, spraying an adhesive, continuously rolling for 5-10 minutes, repeating the operation for 4-8 times, and sieving by using a sieve with 8-10 meshes to obtain spherical granules with the particle diameter of 1.7-2.36 mm.
The ball rolling device is adopted to carry out ball rolling operation on the synthetic zeolite raw powder and the binder, so that the size of spherical particles formed by the mixture is stable and is maintained within 1.7-2.36 mm, and the quality of the prepared spherical 4A molecular sieve is ensured; the rolling ball device adheres the adhesive to the outer surface of the synthetic zeolite, and then the adhesive and the synthetic zeolite can be effectively bonded in the rolling process on the inner cylinder of the ball rolling machine, so that the connection firmness and the adhesion stability between the synthetic zeolite and the adhesive are greatly improved. Meanwhile, the molecular sieve with relatively uniform mass is screened out by virtue of the centrifugal force generated when the rolling ball device rotates, the obtained molecular sieve has uniform mass, the whole adhered adhesive has neat appearance without edges and corners, and the particle surface is uniform, so that the quality of the manufactured molecular sieve is greatly improved.
Preferably, in the fifth step, the temperature of the dryer gradually rises from the feeding direction to the discharging direction, and the dryer is sequentially divided into five temperature zones; the temperature of the first temperature zone is 60 +/-10 ℃; the temperature of the second temperature zone is 70 +/-10 ℃; the temperature of the third temperature zone is 80 +/-10 ℃; the temperature of the fourth temperature zone is 90 +/-10 ℃; the temperature in the fifth temperature zone was 100. + -. 10 ℃.
By adopting the technical scheme, the moisture in the spherical particles formed by the mixture can be slowly emitted from the interior, and the phenomenon that the surfaces of the spherical particles formed by the mixture are cracked due to the fact that the temperature is quickly increased at one time is avoided.
Preferably, in the sixth step, the roasting temperature gradually rises from the feeding direction to the discharging direction of the rotary kiln, and the roasting is divided into eight temperature zones in sequence; the temperature difference between two adjacent temperature areas is controlled to be 60-110 ℃; the temperature of the initial first temperature zone is 100-; the rotary kiln is rotated at a speed of 5-10 rpm.
Mixing the synthetic zeolite raw powder and a binder into a spherical shape, roasting the spherical shape in eight temperature zones, and sintering the spherical shape to obtain the spherical 4A molecular sieve; the molecular sieve is more uniformly activated by the roasting action of the eight temperature zones, so that the condition that the temperature rises too fast at a moment to cause defects inside and on the surface of the molecular sieve and form cracks to influence the product quality can be avoided.
To sum up, the application comprises the following beneficial technical effects:
1. the method adopts the synthetic zeolite raw powder as the raw material, not only has lower cost, but also has uniform size and quality of the finished molecular sieve and has better adsorption capacity and abrasion rate.
2. The optimized mixture of the adhesive and the synthetic zeolite raw powder has high dispersity and ultrafine particle size, and the particle size of the mixture is stabilized within a range by rolling ball operation of the rolling ball device, the rolling ball device adheres the adhesive to the outer surface of the synthetic zeolite, and then the adhesive and the synthetic zeolite can be effectively bonded in the rolling process on the inner cylinder of the rolling ball device, so that the bonding firmness and the bonding stability between the synthetic zeolite and the adhesive are greatly improved.
Drawings
FIG. 1 is a schematic structural diagram of a premixing device in a first embodiment of the present application.
FIG. 2 is a schematic structural diagram of a premixing mechanism in one embodiment of the present application.
Fig. 3 is a schematic structural diagram of a compression mechanism in one embodiment of the present application.
Fig. 4 is a schematic structural diagram of a breaking mechanism in the first embodiment of the present application.
FIG. 5 is a schematic view of a ball-rolling device according to an embodiment of the present invention.
Fig. 6 is a schematic structural diagram of a spray assembly according to an embodiment of the present application.
In the figure, 1, a premixing device; 11. a support; 111. a first mounting layer; 112. a second mounting layer; 1121. a channel; 113. a third mounting layer; 12. a premixing mechanism; 121. a mixing tank body; 122. a screw conveying assembly; 1221. a double helix agitator; 1222. a servo motor; 123. a feed pipe; 1231. sealing the cover; 124. a discharge pipe; 1241. an electromagnetic valve; 13. a compression mechanism; 131. compressing the tube; 132. a first compression member; 1321. a cylinder; 1322. compressing the block; 133. a second compression member; 14. a breaking mechanism; 141. a housing; 142. a crushing roller; 143. rolling a roller; 144. a collecting hopper; 145. a discharge pipe fitting; 1451. a straight pipe; 1452. a control valve; 1453. a telescopic pipe; 15. a ball milling mechanism; 2. a ball rolling device; 21. a bowl body of the ball; 22. a drive mechanism; 221. a support body; 222. connecting columns; 223. a connecting rod; 224. a driven gear; 225. a motor; 226. a driving gear; 23. an adjustment mechanism; 231. a base; 232. an electric pushing cylinder; 24. a liquid material spraying mechanism; 241. a water tank; 2411. a water delivery pipe; 2412. a first ball valve; 242. an inorganic silicon solvent storage tank; 2421. a delivery pipe; 2422. a second ball valve; 243. a centrifugal pump; 2431. a first infusion tube; 2432. a second infusion tube; 244. a spray assembly; 2441. spraying a main pipe; 2442. a pulse valve; 3. a shower head; 31. a hollow sphere; 311. a cavity; 32. a shower pipe; 33. and a spray header.
Detailed Description
The present application is described in further detail below with reference to figures 1-6 and examples.
Examples
Example one
Referring to fig. 1, the equipment required for preparing the professional molecular sieve desiccant of the brake system disclosed by the application comprises a premixing device 1, wherein the premixing device 1 comprises a bracket 11, a premixing mechanism 12, a compression mechanism 13, a breaking mechanism 14 and a ball milling mechanism 15, which are of a three-layer structure, and a first mounting layer 111, a second mounting layer 112 and a third mounting layer 113 are sequentially formed on the bracket 11 from bottom to top; the premixing mechanism 12 is fixedly connected to the third mounting layer 113 and is communicated with the compression mechanism 13; the compressing mechanism 13 is fixedly connected with the second mounting layer 112 and is communicated with the breaking mechanism 14; the breaking mechanism 14 is fixedly connected to the first mounting layer 111 and can be communicated with the ball milling mechanism 15; the ball milling mechanism 15 is arranged on the ground, and the ball milling mechanism 15 is a planetary ball mill.
Referring to fig. 1 and 2, the premixing mechanism 12 includes a mixing tank 121, a screw conveyor assembly 122 rotatably coupled to the inside of the mixing tank 121 for mixing the synthetic zeolite and the binder; one end of the mixing tank body 121 is circumferentially communicated with a feeding pipe 123; the end of the feed pipe 123 is connected with a sealing cover 1231 through threads; a vertical discharge pipe 124 is circumferentially communicated with the bottom of the other end of the mixing tank body 121, and the discharge pipe 124 is communicated with the compression mechanism 13; an electromagnetic valve 1241 is fixedly communicated with the discharge pipe 124; the electromagnetic valve 1241 is located in the circumferential direction of the mixing tank 121.
Referring to fig. 1 and 2, the screw conveyor assembly 122 includes a double screw agitator 1221 rotatably connected to the inside of the mixing tank 121 and a servo motor 1222 for driving the double screw agitator 1221 to rotate, wherein a central axis of the double screw agitator 1221 coincides with a central axis of the mixing tank 121; one end of the double-helix stirrer 1221 is rotatably connected to the mixing tank 121, and the pipe end of the double-helix stirrer 1221, which is positioned outside the mixing tank 121, is fixedly connected to the output shaft of the servo motor 1222 through a coupling; the servo motor 1222 is bolt-fixedly coupled to the third seating layer 113. The servo motor 1222 controls the double screw agitator 1221 to rotate forward and backward, thereby sufficiently mixing the synthetic zeolite and the binder.
Referring to fig. 1 and 3, the compressing mechanism 13 includes a compressing pipe 131, a first compressing member 132, and a second compressing member 133, the first compressing member 132 and the second compressing member 133 being respectively disposed at both sides of a pipe end of the compressing pipe 131 for compressing the synthetic zeolite and the adhesive into a mass; the first compressing member 132 and the second compressing member 133 have the same structure, and taking the first compressing member 132 as an example, the first compressing member 132 includes an air cylinder 1321 and a compressing block 1322, and the compressing block 1322 is fixedly connected to a push rod of the air cylinder 1321; the compression block 1322 is movable in the axial direction of the compression pipe 131; the second mounting layer 112 is provided with a channel 1121 for compressed material to flow to the breaking mechanism 14; the discharge pipe 124 is connected to the compression pipe 131 in the circumferential direction. The first compressing member 132 is located at the left side of the tube end of the compressing tube 131, the second compressing member 133 is located at the right side of the tube end of the compressing tube 131, and the channel 1121 is located between the first compressing member 132 and the compressing tube 131; the connection between the discharge pipe 124 and the compression pipe 131 is located in the circumferential direction of the compression pipe 131 on the side close to the second compression member 133.
The material mixed by the premixing mechanism 12 flows into the compression pipe 131 through the discharge pipe 124, the compression block 1322 of the first compression element 132 is kept still, the air cylinder 1321 of the second compression element 133 is started, the compression block 1322 of the second compression element 133 is driven to move towards the compression block 1322 of the first compression element 132, so that the mixed material is compressed into blocks, then the air cylinder 1321 of the first compression element 132 is started, the compression block 1322 of the first compression element 132 moves leftwards, the air cylinder 1321 of the second compression element 133 is started, and the compression block 1322 of the second compression element 133 pushes the compressed material out of the compression pipe 131 and flows into the crushing mechanism 14 through the passage 1121 for crushing treatment.
Referring to fig. 1 and 4, the crushing mechanism 14 includes a housing 141, a pair of crushing rollers 142 for crushing the compressed material, a pair of crushing rollers 143 for crushing the crushed material, and a collecting hopper 144 for collecting the crushed material, wherein the crushing rollers 142 and the crushing rollers 143 are respectively and fixedly connected to a driving motor for driving them to rotate to crush the material compressed into blocks. The connecting line of the planes of the central axes of the two crushing rollers 142 is a horizontal plane; the connecting line of the planes of the central axes of the two rolling rollers 143 is a horizontal plane; the connecting line of the tangent points of the two crushing rollers 142 and the tangent points of the two rolling rollers 143 is vertical to the surface of the first mounting layer 111; the vertical projections of the crushing roller 142 and the grinding roller 143 both fall within the vertical projection of the collecting hopper 144; the bottom of the collecting hopper 144 is funnel-shaped and is communicated with a discharging pipe fitting 145; the discharge pipe 145 comprises a straight pipe 1451 communicated with the bottom of the collecting hopper 144, and a control valve 1452, preferably a ball valve, is fixedly communicated with the straight pipe 1451; one end of the straight pipe 1451 is connected to the bottom of the collecting hopper 144, and the other end is connected to a telescopic pipe 1453, and the telescopic pipe 1453 can add the material to be ball milled to the ball milling mechanism 15.
Referring to fig. 5, the equipment required for preparing the professional molecular sieve desiccant of the brake system further comprises a rolling ball device 2, wherein the rolling ball device 2 comprises a rolling ball tank body 21, a driving mechanism 22 for driving the rolling ball tank body 21 to rotate around the axial direction of the rolling ball tank body, an adjusting mechanism 23 and a liquid material spraying mechanism 24, and the adjusting mechanism 23 is used for adjusting the inclination angle of the rolling ball tank body 21; the liquid material spraying mechanism 24 is used for spraying liquid materials into the rolling ball tank body 21.
Referring to fig. 5, the driving mechanism 22 comprises a support body 221, a connecting column 222 hinged to the middle of the upper surface of the support body 221, a connecting rod 223, a driven gear 224, a motor 225 and a driving gear 226, wherein one end of the connecting rod 223 is welded to the center of the bottom of the ball tank 21, and the other end of the connecting rod 223 is rotatably connected to the connecting column 222; the driven gear 224 is fixedly connected to the circumferential direction of the connecting rod 223 and meshed with the driving gear 226; the driving gear 226 is fixedly connected to the circumference of the output shaft of the motor 225; the motor 225 is fixedly connected to the circumferential direction of the connection column 222.
Referring to fig. 5, the adjusting mechanism 23 includes a base 231, an electric push cylinder 232; the base 231 is fixedly connected to the ground; the electric pushing cylinder 232 is fixedly connected to the base 231; the push rod of the electric push cylinder 232 is fixedly connected with the column end circumference of the connecting column 222 back to the rolling ball tank body 21.
Referring to fig. 5, the liquid material spraying mechanism 24 includes a water tank 241, an inorganic silicon solvent storage tank 242, a centrifugal pump 243 and a spraying assembly 244, wherein one end of the centrifugal pump 243 is communicated with a first liquid conveying pipe 2431, and the other end is communicated with a second liquid conveying pipe 2432; the water tank 241 is communicated with a water conveying pipe 2411; the water conveying pipe 2411 is communicated with the circumferential direction of the second liquid conveying pipe 2432; a first ball valve 2412 is fixedly communicated with the water delivery pipe 2411; the inorganic silicon solvent storage tank 242 is communicated with a conveying pipe 2421; the conveying pipe 2421 is communicated with the circumferential direction of a second infusion pipe 2432; a second ball valve 2422 is fixedly communicated with the conveying pipe 2421.
Referring to fig. 5 and 6, the spray assembly 244 includes a main spray pipe 2441 and a spray header 3, one end of the main spray pipe 2441 is in threaded communication with the first liquid delivery pipe 2431, the other end of the main spray pipe is in threaded communication with the spray header 3, and the threads are in threaded communication with the wound raw rubber tape to ensure tightness; a pulse valve 2442 is fixedly communicated with the spraying main pipe 2441.
Referring to fig. 5 and 6, the shower head 3 includes a hollow sphere 31, a plurality of shower pipes 32, and a plurality of shower heads 33, the hollow sphere 31 integrally forming a cavity 311; the spray pipe 32 is fixedly connected with the hollow sphere 31; one end of the spray pipe 32 is communicated with the cavity 311; the spray header 33 is communicated with the other end of the spray pipe 32; the spray head 33 faces the interior of the ball jar 21.
A method for preparing a professional molecular sieve desiccant for a brake system by using the equipment comprises the following steps:
step one, preparing synthetic zeolite raw powder; step 1.1, raw material pretreatment: selecting kaolin with the molar ratio of SiO2/Al2O3 of 2.08 for grinding treatment, and screening out the kaolin with the fineness of 13 mu m by using a 1000-mesh screen;
step 1.2, dehydration treatment: roasting the kaolin with the fineness of 13 mu m obtained by screening at 850 ℃ for 3 hours, and dehydrating to obtain metakaolin;
step 1.3, screening: screening metakaolin by using a 1000-mesh screen;
step 1.4, gelation: preparing a sodium hydroxide solution with the concentration of 2.85mol/L, wherein the mass ratio of the amount of the metakaolin to the sodium hydroxide solution in the step 1.2 is 1: 55, adding the metakaolin obtained in the step 1.2 into a sodium hydroxide solution, and stirring and gelling at the temperature of 78 ℃;
step 1.5, aging treatment: transferring the material obtained in the step 1.4 to an environment with the temperature of 20 ℃, and standing for 1 hour;
step 1.6, crystallization treatment; transferring the material obtained in the step 1.5 to an environment with the temperature of 60 ℃, heating to 90 ℃ at the heating rate of 2.5 ℃, preserving the heat for 2.5 hours, and crystallizing to obtain a 4A molecular sieve;
step 1.7, performing suction filtration, washing with 0.1mol of sodium hydroxide until the pH value is 11, and drying at 100 ℃ to obtain 4A molecular sieve raw powder;
step two, uniformly mixing the raw materials: weighing 16kg of 4A molecular sieve raw powder in the first step, weighing 0.48kg of kaolin, 0.24kg of attapulgite, 0.08kg of goat's sweet soil and 0.08kg of bentonite to prepare an adhesive, putting the adhesive into a premixing device 1, mixing and dispersing the 4A molecular sieve raw powder and the adhesive by using a premixing mechanism 12, compressing the mixed and dispersed materials of the premixing mechanism 12 into blocks by using a compression mechanism 13, crushing and grinding the compressed blocks by using a crushing mechanism 14 to obtain high-dispersibility synthetic zeolite raw powder and adhesive mixture, and finally performing ball milling treatment on the high-dispersibility synthetic zeolite raw powder and adhesive mixture by using a planetary ball mill 15 to obtain high-dispersibility synthetic zeolite raw powder and adhesive mixture;
step three, rolling ball treatment: putting the mixture obtained in the step two into a rolling ball device 2 for rolling ball treatment, controlling the rotation speed of a rolling ball tank body 21 to be 60 r/min earlier, atomizing and spraying water on the outer surface of the mixture by using a spraying assembly 244, wherein the water amount is 80ml, continuously rolling for 20min at the rolling ball speed of 75 r/min, then spraying water on the mixture by using the spraying assembly 244, and continuously rolling for 5min after spraying 0.1kg of adhesive (prepared by 0.06kg of kaolin, 0.02kg of attapulgite, 0.01kg of goat's sweet earth and 0.01kg of bentonite) with the water amount of 40ml, and repeating the following operations: spraying water to the mixture by using a spraying assembly 244, wherein the water amount is 40ml, 0.1kg of adhesive (prepared from 0.06kg of kaolin, 0.02kg of attapulgite, 0.01kg of goat's sweet earth and 0.01kg of bentonite) is sprayed on the mixture, the mixture continuously rolls for 5 minutes, after 5 times of repeated operation, the mixture is screened by using a 10-mesh screen, the material which penetrates through the 10-mesh screen is screened by using an 8-mesh screen, and the material intercepted by the 8-mesh screen is taken to obtain spherical granules with the spherical particle diameter of 1.7-2.36 mm;
step four, vibrating and screening, carrying out secondary rolling operation on the spherical granules, atomizing and spraying inorganic silicon solution on the outer surface of the mixture by adopting a spraying assembly 244, wherein the inorganic silicon solvent in the inorganic silicon solution is 3 wt%, the inorganic silicon solution amount is 30ml, continuously rolling for 5 minutes at the rolling speed of 60 revolutions per minute, and repeating the following operations: atomizing and spraying an inorganic silicon solution on the outer surface of the mixture by using a spraying assembly 244, wherein the inorganic silicon solvent in the inorganic silicon solution accounts for 3 wt%, the inorganic silicon solution amount is 30ml, continuously rolling for 5 minutes at a rolling ball speed of 60 r/min, repeatedly performing the operation for 4 times, screening by using a 10-mesh screen, screening the material penetrating through the 10-mesh screen by using an 8-mesh screen, and taking the material intercepted by the 8-mesh screen to obtain spherical granules with the spherical particle diameter of 1.7-2.36 mm;
step five, drying: feeding the material obtained by screening in the step 4 into a dryer, sequentially passing the material through a first drying zone at 60 ℃, a second drying zone at 70 ℃, a third drying zone at 80 ℃, a fourth drying zone at 90 ℃ and a fifth drying zone at 100 ℃, wherein the retention time of each drying zone is 10 mm, drying, and controlling the humidity of the dried molecular sieve to be 31% of the total weight of the molecular sieve;
step six, roasting: feeding the dried material in the fifth step into a roasting furnace, sequentially passing the material through a first roasting area at 110 ℃ for 10min, a second roasting area at 210 ℃ for 5min, a third roasting area at 310 ℃ for 5min, a fourth roasting area at 420 ℃ for 5min, a fifth roasting area at 530 ℃, a sixth roasting area at 640 ℃ for 8min, a seventh roasting area at 750 ℃ for 8min and an eighth roasting area at 850 ℃ for 20min, wherein the rotating speed of the rotary furnace is 8 revolutions per minute;
step seven, screening and heat dissipation: screening the spherical material obtained by roasting in the step six by using a 10-mesh screen to obtain a spherical material with the diameter of 1.7mm, and performing blast heat dissipation treatment to obtain a 4A spherical molecular sieve;
and step eight, putting the 4A spherical molecular sieve obtained in the step seven into a stirring kettle, vacuumizing, taking out, packaging and warehousing.
Example two
The difference between the second embodiment and the first embodiment is that: step 1.1, raw material pretreatment: selecting kaolin with the molar ratio of SiO2/Al2O3 of 2.08, grinding, and sieving with a 600-mesh sieve to obtain the kaolin with the fineness of 23 μm.
EXAMPLE III
The difference between the third embodiment and the first embodiment is that: step 1.1, raw material pretreatment: selecting kaolin with the molar ratio of SiO2/Al2O3 of 2.08 for grinding treatment, and sieving the kaolin with a 1340-mesh sieve to obtain the kaolin with the fineness of 10 mu m.
Example four
The difference between the fourth embodiment and the first embodiment is that: step 1.4, gelation: preparing a sodium hydroxide solution with the concentration of 2.85mol/L, wherein the mass ratio of the amount of the metakaolin to the sodium hydroxide solution in the step 1.3 is 1: 55, adding the metakaolin obtained in the step 1.3 into a sodium hydroxide solution, and stirring the gel at the temperature of 60 ℃.
EXAMPLE five
The difference between the fifth embodiment and the first embodiment is that: step 1.4, gelation: preparing a sodium hydroxide solution with the concentration of 2.85mol/L, wherein the mass ratio of the amount of the metakaolin to the sodium hydroxide solution in the step 1.3 is 1: 55, adding the metakaolin obtained in the step 1.3 into a sodium hydroxide solution, and stirring the gel at a temperature of 68 ℃.
EXAMPLE six
The difference between the sixth embodiment and the first embodiment is that: the adhesive in the step 1 comprises 60% of kaolin, 15% of attapulgite, 20% of sheep's galangal and 5% of bentonite by mass.
EXAMPLE seven
The seventh embodiment differs from the first embodiment in that: the adhesive in the step 1 comprises 60% of kaolin, 25% of attapulgite, 10% of sheep's galangal and 5% of bentonite by mass.
Example eight
The difference between the eighth embodiment and the first embodiment is that: step five, drying: feeding the material obtained by screening in the step 4 into a dryer, sequentially passing the material through a first drying zone at 70 ℃, a second drying zone at 80 ℃, a third drying zone at 90 ℃, a fourth drying zone at 100 ℃ and a fifth drying zone at 110 ℃, wherein the retention time of each drying zone is 10 mm, performing drying treatment, and controlling the humidity of the dried spherical material to be 28% of the total weight of the spherical material, in the ninth embodiment
The ninth embodiment differs from the first embodiment in that: step five, drying: and (3) feeding the material obtained by screening in the step (4) into a dryer, sequentially passing the material through a first drying zone at 75 ℃, a second drying zone at 85 ℃, a third drying zone at 95 ℃, a fourth drying zone at 105 ℃ and a fifth drying zone at 115 ℃, wherein the retention time of each drying zone is 10 mm, and drying, wherein the humidity of the dried spherical material is controlled to be 26% of the total weight of the spherical material.
Comparative example
Comparative example 1
The difference between the first comparative example and the first example is that: natural zeolite is used instead of synthetic zeolite.
Comparative example No. two
The difference between the second comparative example and the first example is that: and step five, after the drying operation, controlling the humidity of the dried spherical material to be 15% of the total weight of the spherical material.
Comparative example No. three
The difference between the second comparative example and the first example is that: and step five, after the drying operation, controlling the humidity of the dried spherical material to be 45% of the total weight of the spherical material.
Performance detection analysis
Test one: performance test subjects: the molecular sieves obtained in examples 1 to 9 were used as sample samples 1 to 9; the molecular sieves obtained in comparative examples 1 to 3 were used as control samples 1 to 3.
The test method comprises the following steps: measuring the static water adsorption performance according to the GB/T6287; the specification in GB/T6286 determines the tap bulk density; the specifications in HG/T2783 are for the resistance to crushing in molecular sieves.
And (2) test II: test object for detecting molecular sieve abrasion rate: the molecular sieves obtained in examples 1 to 9 were used as sample samples 1 to 9; the molecular sieves obtained in comparative examples 1 to 3 were used as control samples 1 to 3.
The test method comprises the following steps:
1. taking about 100 g of a sample, and carrying out concentration division on the sample into two parts by a quartering method, wherein each part is approximately equal to the dosage of an abrasion test: (25. + -. 2) g.
2. Two porcelain crucibles of constant weight m1 (accurate to 0.001 g) were taken which had been fired at 550 ℃. The two samples were poured into test sieves with a pore size of 0.85mm, and the ground material was removed before grinding and transferred to two porcelain crucibles of known quality.
3. The porcelain crucible and the crucible lid (not covered on the crucible) were placed in a box-type resistance furnace and fired at 550 ℃ for 2 hours. The removed porcelain crucible is put into a vacuum drier, and a crucible cover and a positive air drier are immediately covered. Turning on the vacuum pump, turning off the vacuum pump under the condition that the vacuum meter shows that the pressure is less than 1.01 × 103Pa, and cooling to room temperature. The piston on the lid of the vacuum drier was slowly rotated to let the atmosphere slowly pass into the drier, the vacuum drier was opened and m2 (accurate to 0.001 g) was weighed immediately after removing the porcelain crucible.
4. Immediately and respectively loading the samples into two sample grinding cylinders, screwing down the cylinder covers, symmetrically loading the sample grinding cylinders on an abrasion tester, starting the abrasion tester, and rotating 1000 times at the rotating speed of 25 +/-1 times per minute.
5. Taking down the grinding sample cylinder, sieving the sample by using a test sieve of 0.60mm, pouring the sample into the original crucible, and roasting and cooling the ground sample according to the same method of the step 3.
6. The mass m3 of the sample after baking was weighed out for the porcelain crucible and the ground and sieved oversize (to the nearest 0.001 g).
7. The abrasion rate w1 was determined as follows:
in the formula:
m 1-the numerical value of the porcelain crucible (connecting cover) mass, the unit is gram;
m 2-mass value of sample on sieve after sieving and roasting before grinding, in gram;
m 3-the mass value of the sample on the sieve after grinding, sieving and roasting, and the unit is gram; the calculation result is represented to the two last decimal places. The average of the two values was taken as the result of the measurement.
The table shows the results of performance tests of sample Nos. 1 to 9 and test samples Nos. 1 to 3
Table 2 shows the results of measuring the wear rates of the test samples 1 to 9 and the test samples 1 to 3
As can be seen from Table 1, the test samples 1-9 and the control samples 1-3 both had an appearance meeting the requirements of the test, were all off-white, off-white spherical particles, and were free of mechanical impurities. Secondly, the static water adsorption performance, the tap bulk density and the crushing resistance of the test samples 1-9 are all superior to those of the sample samples 1-3, namely the 4A spherical molecular sieve prepared by the method has the advantages of large adsorption quantity, low tap bulk density, large number of openings, large specific surface area and excellent crushing resistance.
As can be seen from table 1, in comparison between the test sample 1 and the test samples 2 and 3, the static water adsorption performance of the test sample 1 is higher than that of the test samples 2 and 3, the synthetic zeolite raw powder prepared from kaolin clay with a fineness of 13 μm is sieved by a 1000-mesh sieve, and the 4A spherical molecular sieve prepared from the synthetic zeolite raw powder is better in static water adsorption performance and larger in specific surface area.
As can be seen from table 1, test sample 1 compared to test samples 4 and 5, the static water adsorption performance of test sample 1 is higher than the static water adsorption performance of test samples 4 and 5, step 1.4, gel: the synthesized zeolite raw powder prepared by gel is stirred at the temperature of 78 ℃, and the 4A spherical molecular sieve prepared by taking the synthesized zeolite raw powder as a raw material has better static water adsorption performance.
As can be seen from table 1, in comparison between the test sample 1 and the test samples 6 and 7, the static water adsorption performance of the test sample 1 is higher than that of the test samples 6 and 7, the binder formula is synthetic zeolite raw powder prepared from 60% by mass of kaolin, 20% by mass of attapulgite, 10% by mass of nacrite and 10% by mass of bentonite, and the static water adsorption performance of the 4A spherical molecular sieve prepared by using the synthetic zeolite raw powder as a raw material is better.
As can be seen from table 1, in comparison between the test sample 1 and the test samples 8 and 9, the static water adsorption performance of the test sample 1 is higher than that of the test samples 8 and 9, and the static water adsorption performance of the 4A spherical molecular sieve prepared by using the synthetic zeolite raw powder as the raw material is better when the synthetic zeolite raw powder prepared by drying the material at 31% moisture in step five is used.
As can be seen from Table 2, the test samples 1 to 9 had lower wear rates than the control samples 1 to 3, and the test samples 1 to 9 had better wear performance. Specifically, the abrasion rate of the test sample 1 is lower than that of the control sample 1, and the abrasion resistance of the 4A spherical zeolite synthesized by using the synthetic zeolite raw material prepared by the method is better; the abrasion rate of the test sample 1 is lower than that of the comparison samples 2 and 3, the synthesized zeolite raw powder prepared by drying the materials in the step five with the moisture of 31 percent has better abrasion resistance of the 4A spherical molecular sieve prepared by taking the synthesized zeolite raw powder as the raw material.
The embodiments of the present invention are preferred embodiments of the present application, and the scope of protection of the present application is not limited by the embodiments, so: all equivalent changes made according to the structure, shape and principle of the present application shall be covered by the protection scope of the present application.
Claims (10)
1. A preparation method of a professional molecular sieve drying agent of a brake system is characterized by comprising the following steps: the method comprises the following steps:
step one, preparing synthetic zeolite raw powder;
step two, uniformly mixing the raw materials: mixing the synthetic zeolite and the binder in the first step according to the mass ratio of (60-80): (2-4) putting the mixture into a premixing device (1) for mixing;
step three, rolling ball treatment: putting the material in the step two into a rolling ball device (2) for rolling ball treatment, wherein the rotating speed of the rolling ball machine is 30-120 r/min;
step four, vibration screening, carrying out secondary rolling operation, and adding 2-6 wt% of inorganic silicon solvent in the secondary rolling process;
step five, drying: drying the material obtained by screening in the step 4 at the temperature of 60-120 ℃, and controlling the humidity of the dried molecular sieve to be 20-40% of the total weight of the molecular sieve;
step six, roasting: feeding the material dried in the step five into a roasting furnace, and roasting for 30-120 minutes at the temperature of 100-850 ℃;
step seven, screening and heat dissipation: screening and radiating the material obtained by roasting in the step six;
and step eight, carrying out vacuum treatment, packaging and warehousing.
2. The preparation method of the professional molecular sieve drying agent for the brake system according to claim 1, wherein the preparation method comprises the following steps: in the first step, the preparation of the synthetic zeolite raw powder specifically comprises the following steps: step 1.1, raw material pretreatment: selecting kaolin with the SiO2/Al2O3 molar ratio of 2.05-2.15, grinding, and sieving with a 600-1340 mesh sieve;
step 1.2, dehydration treatment: roasting and dehydrating the kaolin obtained by screening at the temperature of 650-850 ℃ to obtain metakaolin;
step 1.3, screening: sieving with a 1000-1340 mesh sieve;
step 1.4, gelation: preparing a sodium hydroxide solution with the concentration of 2.45-3.65 mol/L, wherein the mass ratio of the amount of the metakaolin to the sodium hydroxide solution in the step 1.3 is 1: (45-60), adding the metakaolin obtained in the step 1.2 into a sodium hydroxide solution, and stirring and gelling at the temperature of 60-80 ℃;
step 1.5, aging treatment: transferring the material obtained in the step 1.4 to an environment with the temperature of 18-25 ℃, and standing for 1-2 hours;
step 1.6, crystallization treatment; transferring the material obtained in the step 1.5 to an environment with the temperature of 60 +/-3 ℃, heating to 90 +/-1.0 ℃ at the heating speed of 2.5 +/-0.3 ℃, and preserving heat for 2-4 hours;
and step 1.7, carrying out suction filtration and washing until the pH value is 10-12, and drying at 100 ℃ to obtain the 4A molecular sieve raw powder.
3. The preparation method of the professional molecular sieve drying agent for the brake system according to claim 1, wherein the preparation method comprises the following steps: the adhesive in the step 1 comprises 40-60% of kaolin, 10-25% of attapulgite, 10-25% of sheep's galangal and 5-10% of bentonite by mass.
4. The preparation method of the professional molecular sieve drying agent for the brake system according to claim 1, wherein the preparation method comprises the following steps: the premixing device (1) comprises a three-layer bracket (11), a premixing mechanism (12), a compression mechanism (13), a breaking mechanism (14) and a ball milling mechanism (15), wherein the bracket (11) is sequentially provided with a first mounting layer (111), a second mounting layer (112) and a third mounting layer (113) from bottom to top; the premixing mechanism (12) is arranged on the third mounting layer (113) and is communicated with the compression mechanism (13); the compression mechanism (13) is arranged on the second mounting layer (112) and is communicated with the breaking mechanism (14); the smashing mechanism (14) is arranged on the first mounting layer (111) and can be communicated with the ball milling mechanism (15); the ball milling mechanism (15) is arranged on the ground.
5. The method for preparing the professional molecular sieve drying agent for the brake system according to claim 4, wherein the method comprises the following steps: the premixing mechanism (12) comprises a mixing tank body (121) and a spiral conveying assembly (122), wherein the spiral conveying assembly (122) is arranged on the mixing tank body (121) and is used for mixing the synthetic zeolite and the adhesive; one end of the mixing tank body (121) is circumferentially communicated with a feeding pipe (123); the end of the feed pipe (123) is connected with a sealing cover (1231) through threads; a discharge pipe (124) is circumferentially communicated with the other end of the mixing tank body (121); the discharge pipe (124) is communicated with the compression mechanism (13); an electromagnetic valve (1241) is arranged on the discharge pipe (124); the electromagnetic valve (1241) is positioned at the circumference of the mixing tank body (121); the spiral conveying assembly (122) comprises a double-spiral stirrer (1221) which is rotatably connected in the mixing tank body (121) and a servo motor (1222) which drives the double-spiral stirrer (1221) to rotate, and the central axis of the double-spiral stirrer (1221) is overlapped with the central axis of the mixing tank body (121); the pipe end of the double-helix stirrer (1221) positioned at the outer side of the mixing tank body (121) is fixedly connected with the output shaft of the servo motor (1222) through a coupling; the servo motor (1222) is fixedly connected to the third mounting layer (113) through bolts; the compression mechanism (13) comprises a compression pipe (131), a first compression piece (132) and a second compression piece (133), wherein the first compression piece (132) and the second compression piece (133) are respectively arranged at the pipe ends of the compression pipe (131) and are used for compressing the synthetic zeolite and the adhesive into blocks; the first compression piece (132) and the second compression piece (133) are identical in structure; the first compression piece (132) comprises an air cylinder (1321) and a compression block (1322), and the compression block (1322) is fixedly connected to a push rod of the air cylinder (1321); the compression block (1322) can move along the axial direction of the compression pipe (131); the second mounting layer (112) is provided with a channel (1121) for compressed materials to flow to the breaking mechanism (14); the discharge pipe (124) is communicated with the circumferential direction of the compression pipe (131).
6. The method for preparing the professional molecular sieve drying agent for the brake system according to claim 5, wherein the method comprises the following steps: the crushing mechanism (14) comprises a shell (141), a pair of crushing rollers (142) for crushing the compressed materials, a pair of grinding rollers (143) for grinding the crushed materials and a collecting hopper (144) for collecting the ground materials, wherein the connecting line of the planes of the central axes of the two crushing rollers (142) is a horizontal plane; the connecting line of the planes of the central axes of the two rolling rollers (143) is a horizontal plane; the connecting line of the tangent points of the two crushing rollers (142) and the tangent points of the two rolling rollers (143) is vertical to the surface of the first mounting layer (111); the vertical projections of the crushing roller (142) and the rolling roller (143) fall in the vertical projection of the collecting hopper (144); the bottom of the collecting hopper (144) is funnel-shaped and is communicated with a discharging pipe fitting (145); the discharge pipe fitting (145) comprises a straight pipe (1451) communicated with the bottom of the collecting hopper (144), a control valve (1452) arranged on the straight pipe (1451) and an extension pipe (1453) communicated with the straight pipe (1451), wherein the extension pipe (1453) can add grinding materials to be ball-milled to the ball-milling mechanism (15); the ball milling mechanism (15) is a planetary ball mill.
7. The preparation method of the professional molecular sieve drying agent for the brake system according to claim 1, wherein the preparation method comprises the following steps: the rolling ball device (2) comprises a rolling ball tank body (21), a driving mechanism (22) for driving the rolling ball tank body (21) to rotate around the axial direction of the rolling ball tank body, an adjusting mechanism (23) and a liquid material spraying mechanism (24), wherein the adjusting mechanism (23) is used for adjusting the inclination angle of the rolling ball tank body (21); the liquid material spraying mechanism (24) is used for spraying liquid materials into the rolling ball tank body (21); the driving mechanism (22) comprises a support body (221), a connecting column (222) hinged to the middle of the support body (221), a connecting rod (223), a driven gear (224), a motor (225) and a driving gear (226), wherein one end of the connecting rod (223) is welded at the center of the bottom of the rolling ball tank body (21), and the other end of the connecting rod is rotatably connected to the connecting column (222); the driven gear (224) is fixedly connected to the circumferential direction of the connecting rod (223) and meshed with the driving gear (226); the driving gear (226) is fixedly connected to the circumferential direction of the output shaft of the motor (225); the motor (225) is fixedly connected to the circumferential direction of the connecting column (222); the adjusting mechanism (23) comprises a base (231) and an electric pushing cylinder (232); the base (231) is fixedly connected to the ground; the electric pushing cylinder (232) is fixedly connected to the base (231); a push rod of the electric pushing cylinder (232) is fixedly connected to the column end circumference of the connecting column (222) back to the rolling ball tank body (21); the liquid material spraying mechanism (24) comprises a water tank (241), an inorganic silicon solvent storage tank (242), a centrifugal pump (243) and a spraying assembly (244), wherein one end of the centrifugal pump (243) is communicated with a first liquid conveying pipe (2431), and the other end of the centrifugal pump (243) is communicated with a second liquid conveying pipe (2432); the water tank (241) is communicated with a water delivery pipe (2411); the water delivery pipe (2411) is communicated with the circumference of the second liquid delivery pipe (2432); a first ball valve (2412) is arranged on the water delivery pipe (2411); the inorganic silicon solvent storage tank (242) is communicated with a conveying pipe (2421); the conveying pipe (2421) is communicated with the circumferential direction of a second infusion pipe (2432); a second ball valve (2422) is arranged on the conveying pipe (2421); the spraying assembly (244) comprises a spraying main pipe (2441) and a spraying head (3), one end of the spraying main pipe (2441) is communicated with the first liquid conveying pipe (2431) in a threaded manner, the other end of the spraying main pipe (2441) is communicated with the spraying head (3), and a pulse valve (2442) is arranged on the spraying main pipe (2441); the spray header (3) comprises a hollow sphere (31), a plurality of spray pipes (32) and a plurality of spray headers (33), and the hollow sphere (31) is integrally formed with a cavity (311); the spray pipe (32) is fixedly connected with the hollow sphere (31); one end of the spray pipe (32) is communicated with the cavity (311); the spray header (33) is communicated with the other end of the spray pipe (32); the spray head (33) faces the interior of the rolling ball tank body (21).
8. The method for preparing the professional molecular sieve drying agent for the brake system according to claim 7, wherein the method comprises the following steps: in step three, the rolling ball is operated in a specific way as follows: adding the material obtained in the second step into the rolling ball device (2) under the rotation of 60 revolutions per minute, spraying water on the outer surface of the material obtained in the second step, continuously rolling for 20-25 minutes at the rolling ball speed of 60-120 revolutions per minute, then spraying water again and spraying adhesive, continuously rolling for 5-10 minutes, and repeating the following operations: spraying water on the outer surface of the material obtained in the step two, spraying an adhesive, continuously rolling for 5-10 minutes, repeating the operation for 4-8 times, and sieving by using a sieve with 8-10 meshes to obtain spherical granules with the particle diameter of 1.7-2.36 mm.
9. The preparation method of the professional molecular sieve drying agent for the brake system according to claim 1, wherein the preparation method comprises the following steps: in the fifth step, the temperature of the dryer gradually rises from the feeding direction to the discharging direction, and the dryer is sequentially divided into five temperature zones; the temperature of the first temperature zone is 60 +/-10 ℃; the temperature of the second temperature zone is 70 +/-10 ℃; the temperature of the third temperature zone is 80 +/-10 ℃; the temperature of the fourth temperature zone is 90 +/-10 ℃; the temperature in the fifth temperature zone was 100. + -. 10 ℃.
10. The method for preparing the professional molecular sieve drying agent for the brake system according to claim 9, wherein the method comprises the following steps: in the sixth step, the temperature of the roasting is gradually increased from the feeding direction to the discharging direction of the rotary furnace, and the roasting is sequentially divided into eight temperature zones; the temperature difference between two adjacent temperature areas is controlled to be 60-110 ℃; the temperature of the initial first temperature zone is 100-; the rotary kiln is rotated at a speed of 5-10 rpm.
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Cited By (3)
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CN113264537A (en) * | 2021-04-21 | 2021-08-17 | 南京永成分子筛有限公司 | Preparation method of efficient NA-X type molecular sieve, spraying equipment and using method of spraying equipment |
CN113578261A (en) * | 2021-08-11 | 2021-11-02 | 南京荣运昌化工有限公司 | Production equipment and preparation method of hollow glass molecular sieve with low nitrogen absorption |
CN114669276A (en) * | 2022-02-16 | 2022-06-28 | 杭州远烨新材料有限公司 | Production process of molecular sieve desiccant |
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CN101406825A (en) * | 2008-11-07 | 2009-04-15 | 中南大学 | Method for synthesizing 4A molecular sieve drier using kaoline |
CN109485058A (en) * | 2018-12-11 | 2019-03-19 | 中国地质科学院郑州矿产综合利用研究所 | Preparation method of binder-free LSX molecular sieve |
CN111167404A (en) * | 2020-01-10 | 2020-05-19 | 上海航中实业有限公司 | Molecular sieve of commercial vehicle brake system and preparation method thereof |
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CN101406825A (en) * | 2008-11-07 | 2009-04-15 | 中南大学 | Method for synthesizing 4A molecular sieve drier using kaoline |
CN109485058A (en) * | 2018-12-11 | 2019-03-19 | 中国地质科学院郑州矿产综合利用研究所 | Preparation method of binder-free LSX molecular sieve |
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CN113264537A (en) * | 2021-04-21 | 2021-08-17 | 南京永成分子筛有限公司 | Preparation method of efficient NA-X type molecular sieve, spraying equipment and using method of spraying equipment |
CN113578261A (en) * | 2021-08-11 | 2021-11-02 | 南京荣运昌化工有限公司 | Production equipment and preparation method of hollow glass molecular sieve with low nitrogen absorption |
CN113578261B (en) * | 2021-08-11 | 2023-05-23 | 南京荣运昌化工有限公司 | Production equipment of hollow glass molecular sieve with low nitrogen absorption and preparation method thereof |
CN114669276A (en) * | 2022-02-16 | 2022-06-28 | 杭州远烨新材料有限公司 | Production process of molecular sieve desiccant |
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Application publication date: 20201211 |