CN114540559A - Application of molecular sieve material in preparation of leather - Google Patents
Application of molecular sieve material in preparation of leather Download PDFInfo
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- CN114540559A CN114540559A CN202210126456.7A CN202210126456A CN114540559A CN 114540559 A CN114540559 A CN 114540559A CN 202210126456 A CN202210126456 A CN 202210126456A CN 114540559 A CN114540559 A CN 114540559A
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- leather
- molecular sieve
- sieve material
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- C—CHEMISTRY; METALLURGY
- C14—SKINS; HIDES; PELTS; LEATHER
- C14C—CHEMICAL TREATMENT OF HIDES, SKINS OR LEATHER, e.g. TANNING, IMPREGNATING, FINISHING; APPARATUS THEREFOR; COMPOSITIONS FOR TANNING
- C14C11/00—Surface finishing of leather
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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
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0056—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the compounding ingredients of the macro-molecular coating
- D06N3/0063—Inorganic compounding ingredients, e.g. metals, carbon fibres, Na2CO3, metal layers; Post-treatment with inorganic compounds
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/12—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins
- D06N3/14—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins with polyurethanes
- D06N3/141—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins with polyurethanes mixture of two or more polyurethanes in the same layer
Abstract
The invention relates to application of a molecular sieve material in preparing leather. The silicon-aluminum ratio of the molecular sieve material is more than or equal to 35. The molecular sieve material has good adsorption effect on VOCs (volatile organic compounds) in leather, such as aldehydes and ketones, aromatic hydrocarbons, halogenated hydrocarbons, alkanes and alcohol ether esters. By adding the material into leather raw materials or products, the content of VOCs can be reduced by more than 90%, and the effect is extremely obvious. Meanwhile, the material has good compatibility with leather raw materials or products such as cow leather, sheep leather, buff leather, artificial leather, synthetic leather and the like, and the physical and mechanical strength of the leather is not obviously reduced after the material is added.
Description
Technical Field
The invention relates to application of a molecular sieve material in preparing leather.
Background
Leather is used as a fabric in leather, and the content of Volatile Organic Compounds (VOCs) becomes a key quality index of products due to the smell and toxicity of the VOCs.
In order to adsorb VOCs in leather, an adsorbing material with excellent performance is needed. On one hand, the adsorbing material needs to have a multi-stage pore channel structure, and can effectively adsorb VOCs molecules with different diameters. On the other hand, the adsorbing material has good compatibility with leather, does not damage the physical and mechanical strength of the leather, and does not corrode the leather.
The molecular sieve is used as an inert porous inorganic material, has developed pore passages, low chemical activity and good compatibility with leather, and therefore has a good effect on adsorbing the VOCs in the leather.
Disclosure of Invention
The invention firstly provides the application of the molecular sieve material in the preparation of leather.
The inventor researches and discovers that the process flow of the leather from the raw material to the finished product is long, and after the finished product is prepared, organic matters are dispersed in the leather by adding a plurality of organic auxiliary materials. Therefore, the adsorption difficulty of VOCs gases such as aldehydes, ketones, aromatic hydrocarbons, halogenated hydrocarbons, alkanes, alcohol ether esters and the like in the leather is high, and the release period is long. The inventors tried adding a low silica alumina ratio molecular sieve (e.g., MFI) to leather for adsorption of VOCs and found that the low silica alumina ratio molecular sieve had poor adsorption and compatibility with leather. On the basis of a great deal of research, the inventor unexpectedly finds that the molecular sieve material with higher silicon-aluminum ratio is particularly suitable for being added into leather to adsorb VOCs, and has good adsorption effect and good compatibility with the leather. Specifically, the Si/Al ratio of the molecular sieve material is more than or equal to 35. Researches show that the molecular sieve has a developed pore channel structure, and VOCs enter the pore channel and are intercepted in a shape-selective manner, so that a better adsorption effect is realized.
Further, the silicon-aluminum ratio of the molecular sieve material is 35- ∞.
According to the embodiment of the invention, the silicon-aluminum ratio of the molecular sieve material is 35-1880 or 38-1880, such as 35, 38, 38.88, 39, 40, 50, 60, 100, 1000, 1500, 1800, 1879.15 and 1880.
The silicon-aluminum ratio refers to the ratio of the mass of alumina content to silica content in the molecular sieve.
Further, the diameter of the molecular sieve material is less than or equal to 200 microns. Specifically, the molecular sieve material has a diameter of 0.5 to 190 microns.
The diameter of the molecular sieve material of the present invention is the average diameter of the particles of the constituent up to a plurality of molecular sieves.
In some examples, the diameter of the molecular sieve material is detected using a laser particle sizer. The detection method of the diameter can refer to GB/T19077.1-2008, GB/T15445.2-2006 and GB/T19627-.
Further, the molecular sieve material has a particle size of 0.1 micron or greater.
According to an embodiment of the invention, the molecular sieve material has a particle size of 0.1 to 8 microns, such as 0.36 to 6.25 microns.
According to an embodiment of the present invention, more than 90% of the molecular sieve material has a particle size below 2 μm.
The particle size of the invention is the diameter of a single crystal of the molecular sieve.
In some examples, the particle size of the molecular sieve material is detected using a laser particle sizer.
Further, the molecular sieve material is organophilic and hydrophobic.
Further, the molecular sieve material contains a plurality of pores, including microporous and mesoporous pores.
Further, the molecular sieve material is not corrosive and does not destroy the physical mechanical strength of the leather.
Further, the molecular sieve material has an adsorption capacity for VOCs in the media at approximately one atmosphere of pressure.
Further, the molecular sieve material has one or more of the structures MFI or BEA.
Further, the molecular sieve material structure may include one or more of FAU, FER, MOR, MWW, MCM, SBA, etc., and basic information about zeolites may be obtained from the International Zeolite Association and corresponding Web site (http:// www.
According to the application, the molecular sieve material is used for adsorbing VOCs gas in leather, and specifically comprises one or more of aldehydes and ketones, aromatic hydrocarbons, halogenated hydrocarbons, alkanes, alcohol ether esters and the like.
According to the above application, the leather includes leather raw materials such as cow leather, sheep leather, buff leather, artificial leather, synthetic leather and the like, and leather products.
Further, the addition amount of the molecular sieve material in the leather is between 0.01 wt% and 25 wt% (based on the total weight of the leather).
According to the invention, the porous material molecular sieve is added into the leather for absorbing VOCs for the first time, so that the adsorption effect is good and the application range is wide.
The invention also provides leather containing the molecular sieve material. For example, in an amount of 0.01 wt% to 25 wt% (based on the total weight of the leather).
In some examples, the leather is PVC artificial leather, and the components thereof include PVC resin, heat stabilizer, foaming agent, heat stabilizer, and plasticizer, or further include pigment. Specifically, the components include polyvinyl chloride resin, dioctyl phthalate, dibutyl phthalate, chlorinated paraffin, barium stearate, lead stearate, cadmium stearate, zinc stearate, calcium carbonate, azodicarbonamide, or further include a pigment. A typical formulation for the leather can be seen in table 1 below. The leather is suitable for adding MFI molecular sieve, and the silicon-aluminum ratio is 1850-1880 (for example 1879.15); the particle size of the molecular sieve material is 0.1-8 μm, and more than 90% of the particles are less than 2 μm. The addition amount of the molecular sieve material in the leather is between 0.3 and 3 weight percent (based on the total weight of the leather).
In some examples, the leather is a PVC foam layer, the components of which include plasticizers, stabilizers, color pastes, foaming agents, and resins, or further include pigments. Specifically, the components include polyvinyl chloride resin, dioctyl phthalate, dibutyl phthalate, chlorinated paraffin, barium stearate, lead stearate, cadmium stearate, zinc stearate, calcium carbonate, azodicarbonamide, or further include a pigment. A typical formulation for the leather can be seen in table 1 below. The leather is suitable for adding MFI molecular sieve, and the silicon-aluminum ratio is 1850-1880 (for example 1879.15); the particle size of the molecular sieve material is 0.1-8 μm, and more than 90% of the particles are less than 2 μm. The addition amount of the molecular sieve material in the leather is between 0.3 wt% and 3 wt% (based on the total weight of the leather).
In some examples, the leather is PU artificial leather, and its components include PU resin and auxiliaries (made into polyurethane resin slurry) such as foaming agent, surfactant, and the like. Specifically, the components comprise waterborne polyurethane, aliphatic waterborne polyurethane, fluff powder, an associated thickener, a defoaming agent, a wetting and leveling agent and water. A typical formulation for the leather can be seen in table 1 below. The leather is suitable for adding BEA molecular sieve, and the silicon-aluminum ratio is 35-40 (for example 38.88); the particle size of the molecular sieve material is 0.1-8 μm, and more than 90% of the particles are less than 2 μm. The addition amount of the molecular sieve material in the leather is between 0.01 and 0.1 weight percent (based on the total weight of the leather).
The invention also provides a preparation method of the leather, which comprises the step of adding the molecular sieve material in the leather preparation process.
In some embodiments, leather may be prepared by calendering or coating.
The molecular sieve material selected by the invention contains a multi-stage pore channel structure, and can effectively adsorb VOCs molecules with different diameters. On the other hand, the adsorbing material is an inert porous inorganic material, has developed pore passages, low chemical activity and good compatibility with leather, does not damage the physical and mechanical strength of the leather, and is a leather VOCs adsorbing material with excellent performance.
Drawings
FIG. 1: the molecular sieve X-ray diffraction of the embodiment of the invention detects the topological structure of the molecular sieve.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention. The examples do not show the specific techniques or conditions, according to the technical or conditions described in the literature in the field, or according to the product specifications. The reagents or instruments used are conventional products available from regular distributors, not indicated by the manufacturer.
The following MFI molecular sieves (No. 1#), MFI molecular sieves (No. 2#), and BEA molecular sieves were provided by Shandong China functional materials, Inc., and their preparation methods are shown in CN108862311A and CN 110482565A.
Comparative example 1
According to the formula of the PVC artificial leather (shown in Table 1), the required PVC resin is mixed with auxiliary agents such as a heat stabilizer, a foaming agent, a heat stabilizer and the like, then softening materials such as a plasticizer and the like are added, the mixture is uniformly mixed on a calender, and calendering are carried out, so that the PVC artificial leather is obtained, namely a sample 1.
Example 1
According to the formula of the PVC artificial leather (same as the formula of the comparative example 1), the required PVC resin, heat stabilizer, foaming agent, heat stabilizer and other additives and 0.3 mass percent of MFI molecular sieve (numbered 1#), wherein the topological structure of the molecular sieve is MFI, the silicon-aluminum ratio is 1879.15, then softening materials such as plasticizer and the like are added, the materials are uniformly mixed on a calender, and calendering are carried out, so that the PVC artificial leather added with the molecular sieve is obtained, namely a sample 2.
Comparative example 2
According to the formula of the raw materials of the PVC foaming layer (shown in Table 1), accurately metering various raw materials, adding a plasticizer, a stabilizer, a color paste, a foaming agent, resin and the like, uniformly mixing and stirring to prepare slurry for the foaming layer, coating the slurry on a carrier by a material carrying roller, feeding the slurry into an oven to enable the slurry to be attached to base cloth, drying for the second time to plasticize or foam, discharging the slurry out of the oven, cooling, and peeling from the carrier to obtain a product, namely a sample 3.
Example 2
Accurately metering various raw materials according to a PVC foaming layer material formula (same as the comparative example 2), adding a plasticizer, a stabilizer, a color paste, a foaming agent, resin and a 3% MFI molecular sieve (numbered 1#), wherein the molecular sieve has an MFI topological structure and a silicon-aluminum ratio of 1879.15, uniformly mixing and stirring to prepare a foaming layer slurry, coating the slurry on a carrier by a material carrying roller, allowing the slurry to be attached to base cloth in an oven, drying for the second time, plasticizing or foaming, taking out of the oven for cooling, and peeling off the carrier to obtain a product, namely a sample 4.
Comparative example 3
According to the PU artificial leather formulation (as shown in table 1). The required PU resin is mixed with auxiliary agents such as foaming agent, surfactant and the like to form polyurethane resin slurry, a base blank is prepared by a wet production process, and then dry transfer veneering is adopted to laminate the skin membrane fabric and the base blank, so that a sample 5 is obtained.
Example 3
According to a formula of PU artificial leather (same as that of a comparative example 3), required PU resin, auxiliary agents such as a foaming agent and a surfactant and a BEA molecular sieve with the mass fraction of 0.01% are mixed to form polyurethane resin slurry, wherein the molecular sieve has a topological structure of BEA and a silicon-aluminum ratio of 38.88, a base blank is prepared through a wet production process, and then dry transfer veneering is adopted to laminate a skin membrane fabric and the base blank to obtain a sample 6.
Comparative example 4
According to the formula of the PVC artificial leather (same as that of comparative example 1), required PVC resin, heat stabilizer, foaming agent, heat stabilizer and other auxiliaries and 0.3 mass percent of MFI molecular sieve (serial number is No. 2), wherein the topological structure of the molecular sieve is MFI, the silicon-aluminum ratio is 30.77, then softening materials such as plasticizer and the like are added, the materials are uniformly mixed on a calender, and calendering are carried out, so that the PVC artificial leather added with the molecular sieve, namely sample 7, is obtained.
TABLE 1 leather formulation
Examples of the experiments
The above MFI molecular sieves (No. 1), BEA molecular sieves and MFI molecular sieves (No. 2) were subjected to X-ray fluorescence spectrum analysis to detect the silica and alumina fractions of the molecular sieves, and the silica/alumina ratios were calculated as 1879.15, 38.88 and 30.77, respectively, after converting the fractions into the amounts of substances (see Table 2). The numerical value of the laser particle size analyzer shows (see table 3), the particle size of the MFI molecular sieve (No. 1#) molecular sieve material is 0.1-8 μm, and more than 90% of the particle size is less than 2 μm. Meanwhile, BET data of the molecular sieve material show that (shown in Table 4) the material is a hierarchical pore material with developed pore channels and has two pore channel structures of micropores and mesopores, so that the material has good adsorption selectivity on large-molecule and small-molecule VOCs. The molecular sieve topology can be analyzed by X-ray diffraction spectroscopy as MFI and BEA (fig. 1). In addition, toluene and water were adsorbed by the molecular sieve material (table 5), which shows that the molecular sieve has a toluene adsorbing capacity much higher than that of water, and is a relatively organophilic and hydrophobic material.
Through the preparation method, 7 groups of leather materials are obtained, Volatile Organic Compounds (VOCs) in the leather are determined by adopting a headspace-gas chromatography (HS-GC) method, and the content of the VOCs in a series of samples is calculated.
The detection method comprises placing the sample into a headspace bottle, heating at 120 deg.C for 5 hr, sucking out VOCs volatilized from leather by injector, and injecting into gas chromatography for analysis. Acetone is used for quantitative calibration of gas chromatography area, each chromatographic peak in a chromatogram shows a VOCs substance, the total area of VOCs is calculated and converted into the content of VOCs, quantitative analysis is realized, VOCs analysis is carried out on samples of examples and comparative examples, and adsorption data are shown in Table 7.
Finally, the strength test (table 6) and the content test (table 7) of the VOCs are carried out on the prepared leather sample, the MFI molecular sieve (with the number of 1#) and the BEA molecular sieve are added, all the strength parameters of the three types of leather are not obviously changed, and the content of the VOCs is respectively and rapidly reduced by 95.8 percent, 95.5 percent and 96.25 percent, so that the prepared leather sample has good leather compatibility and VOCs adsorption performance. However, the MFI molecular sieve (No. 2) with low silicon-aluminum ratio has no difference from the MFI molecular sieve (No. 1) in all other indexes except the silicon-aluminum ratio, but the adsorption efficiency of VOCs is only 48.8%, which is much lower than that of the MFI molecular sieve (No. 1).
Therefore, the molecular sieve material is used for absorbing VOCs in leather, and has good market application prospect.
TABLE 2X-ray fluorescence Spectroscopy
TABLE 3 MFI molecular sieves (numbered # 1) laser particle size data
TABLE 4 molecular sieve BET data (specific surface area, pore internal diameter, pore volume)
TABLE 5 molecular sieves toluene Water adsorption
Sample (I) | Toluene adsorption Rate/% | Water adsorption rate/%) |
MFI molecular sieve (number 1#) | 12.15 | 1.12 |
MFI molecular sieve (number 1#) | 11.85 | 1.53 |
BEA | 20.33 | 10.87 |
TABLE 6 mechanical Strength of samples prepared
Strength of | Sample 1 | Sample 2 | Sample 3 | Sample No. 4 | Sample No. 5 | Sample No. 6 | Sample 7 |
Tensile Strength/N | 158.93 | 159.04 | 127.87 | 127.46 | 263.44 | 263.49 | 159.37 |
Tear Strength/N | 83.22 | 83.27 | 65.11 | 64.88 | 27.05 | 26.98 | 83.1 |
Suture Strength/N | 199.57 | 200.55 | 189.25 | 189.18 | 184.26 | 184.30 | 199.93 |
Peel strength/N | 14.71 | 14.73 | 15.68 | 15.71 | 18.70 | 18.66 | 14.93 |
Table 7 testing of VOCs content of prepared samples
Finally, it should be noted that: the above examples are only for illustrating the present invention and not for limiting the technical solutions described in the present invention, and the applicable leather raw material or leather products are not limited to the examples, therefore, although the present invention has been described in detail by referring to the above examples, it should be understood by those skilled in the art that the present invention can be modified or substituted equally without departing from the spirit and scope of the present invention, and all technical solutions and modifications thereof that do not depart from the spirit and scope of the present invention should be covered in the claims of the present invention.
Claims (10)
1. The application of molecular sieve material in preparing leather; wherein the silicon-aluminum ratio of the molecular sieve material is more than or equal to 35.
2. Use according to claim 1, wherein the molecular sieve material has a silica to alumina ratio of from 35 to 1880, optionally from 38 to 1880.
3. The use of claim 1, wherein the molecular sieve material has a silica to alumina ratio of 35, 38, 38.88, 39, 40, 50, 60, 100, 1000, 1500, 1800, 1879.15, or 1880.
4. The use of any of claims 1-3, wherein the molecular sieve material has a diameter of 200 microns or less; optionally, the molecular sieve material has a diameter of 0.5 to 190 microns.
5. The use of any one of claims 1-4, wherein the molecular sieve material has a particle size of 0.1 micron or greater; optionally, the molecular sieve material has a particle size of 0.1 to 8 microns, optionally 0.36 to 6.25 microns.
6. Use according to any one of claims 1 to 5, wherein 90% or more of the molecular sieve material has a particle size below 2 μm.
7. The use according to any one of claims 1 to 6, wherein the molecular sieve material is organophilic and hydrophobic; and/or the presence of a gas in the gas,
the molecular sieve material contains a plurality of pores including micropores and mesopores; and/or the presence of a gas in the gas,
the molecular sieve material is not corrosive and does not destroy the physical and mechanical strength of leather; and/or the presence of a gas in the gas,
at approximately one atmosphere, the molecular sieve material has an adsorption capacity for VOCs in the medium; and/or the presence of a gas in the gas,
the molecular sieve material has one or more of the structures MFI or BEA.
8. Use according to any one of claims 1 to 7, wherein the leather comprises leather raw materials and leather products; optionally, the leather raw material comprises cow leather, sheep leather, suede leather, artificial leather, synthetic leather.
9. Leather, characterized by containing a molecular sieve material; the molecular sieve material is the same as the molecular sieve material of any one of claims 1 to 7; optionally, the content of the molecular sieve material in the leather is 0.01 wt% to 25 wt%.
10. A method for preparing leather is characterized by comprising the steps of adding a molecular sieve material in the leather preparation process; the molecular sieve material is the same as the molecular sieve material of any one of claims 1 to 7.
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CN110482565A (en) * | 2019-09-11 | 2019-11-22 | 江苏国瓷天诺新材料科技股份有限公司 | A method of utilizing total silicon Beta crystallization mother liquor synthesizing low silicon aluminium ratio Beta molecular sieve |
CN112371082A (en) * | 2020-11-09 | 2021-02-19 | 天长市润源催化剂有限公司 | Synthesis method of molecular sieve based on reduction of VOC content in finished leather |
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WO2017012240A1 (en) * | 2015-07-22 | 2017-01-26 | 江苏国信复合材料科技股份有限公司 | Nanometer artificial leather and manufacturing method therefor |
CN107747233A (en) * | 2017-10-27 | 2018-03-02 | 佛山威明塑胶有限公司 | A kind of PVC artificial leather of low smell and preparation method thereof |
CN109248672A (en) * | 2018-06-28 | 2019-01-22 | 霍尼韦尔特性材料和技术(中国)有限公司 | A kind of composite material and preparation method and application |
CN108842010A (en) * | 2018-07-05 | 2018-11-20 | 西安理工大学 | The method for preparing white vollyball leather |
CN108862311A (en) * | 2018-08-31 | 2018-11-23 | 江苏国瓷天诺新材料科技股份有限公司 | A kind of preparation method of the high silica ZSM-5 molecular sieve for VOCs degradation |
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CN112371082A (en) * | 2020-11-09 | 2021-02-19 | 天长市润源催化剂有限公司 | Synthesis method of molecular sieve based on reduction of VOC content in finished leather |
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