CN115028177A - Hydrophobic superfine modified anhydrous sodium sulphate and preparation method thereof - Google Patents
Hydrophobic superfine modified anhydrous sodium sulphate and preparation method thereof Download PDFInfo
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- anhydrous sodium
- sodium sulphate
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- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 title claims abstract description 318
- 229910052938 sodium sulfate Inorganic materials 0.000 title claims abstract description 156
- 235000011152 sodium sulphate Nutrition 0.000 title claims abstract description 156
- 230000002209 hydrophobic effect Effects 0.000 title claims abstract description 82
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- OVBPIULPVIDEAO-LBPRGKRZSA-N folic acid Chemical compound C=1N=C2NC(N)=NC(=O)C2=NC=1CNC1=CC=C(C(=O)N[C@@H](CCC(O)=O)C(O)=O)C=C1 OVBPIULPVIDEAO-LBPRGKRZSA-N 0.000 claims abstract description 66
- RSKGMYDENCAJEN-UHFFFAOYSA-N hexadecyl(trimethoxy)silane Chemical compound CCCCCCCCCCCCCCCC[Si](OC)(OC)OC RSKGMYDENCAJEN-UHFFFAOYSA-N 0.000 claims abstract description 40
- CTENFNNZBMHDDG-UHFFFAOYSA-N Dopamine hydrochloride Chemical compound Cl.NCCC1=CC=C(O)C(O)=C1 CTENFNNZBMHDDG-UHFFFAOYSA-N 0.000 claims abstract description 36
- 229960001149 dopamine hydrochloride Drugs 0.000 claims abstract description 35
- 235000019152 folic acid Nutrition 0.000 claims abstract description 33
- 239000011724 folic acid Substances 0.000 claims abstract description 33
- OVBPIULPVIDEAO-UHFFFAOYSA-N N-Pteroyl-L-glutaminsaeure Natural products C=1N=C2NC(N)=NC(=O)C2=NC=1CNC1=CC=C(C(=O)NC(CCC(O)=O)C(O)=O)C=C1 OVBPIULPVIDEAO-UHFFFAOYSA-N 0.000 claims abstract description 32
- 229960000304 folic acid Drugs 0.000 claims abstract description 32
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000004094 surface-active agent Substances 0.000 claims description 54
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 36
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 34
- 238000003756 stirring Methods 0.000 claims description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 29
- FYFFGSSZFBZTAH-UHFFFAOYSA-N methylaminomethanetriol Chemical compound CNC(O)(O)O FYFFGSSZFBZTAH-UHFFFAOYSA-N 0.000 claims description 19
- 238000000227 grinding Methods 0.000 claims description 18
- 229910052757 nitrogen Inorganic materials 0.000 claims description 18
- 238000009210 therapy by ultrasound Methods 0.000 claims description 14
- 239000011259 mixed solution Substances 0.000 claims description 12
- LENZDBCJOHFCAS-UHFFFAOYSA-N tris Chemical compound OCC(N)(CO)CO LENZDBCJOHFCAS-UHFFFAOYSA-N 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000005507 spraying Methods 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 2
- 238000006482 condensation reaction Methods 0.000 abstract description 10
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 5
- 238000010521 absorption reaction Methods 0.000 abstract description 5
- 229920001690 polydopamine Polymers 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 4
- 238000005054 agglomeration Methods 0.000 abstract description 3
- 230000002776 aggregation Effects 0.000 abstract description 3
- 239000002086 nanomaterial Substances 0.000 abstract description 3
- 238000001953 recrystallisation Methods 0.000 abstract description 3
- 230000004048 modification Effects 0.000 description 7
- 238000012986 modification Methods 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 239000012535 impurity Substances 0.000 description 4
- 238000006116 polymerization reaction Methods 0.000 description 4
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000006087 Silane Coupling Agent Substances 0.000 description 2
- 239000007853 buffer solution Substances 0.000 description 2
- 239000012159 carrier gas Substances 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 239000010446 mirabilite Substances 0.000 description 2
- 238000003541 multi-stage reaction Methods 0.000 description 2
- RSIJVJUOQBWMIM-UHFFFAOYSA-L sodium sulfate decahydrate Chemical compound O.O.O.O.O.O.O.O.O.O.[Na+].[Na+].[O-]S([O-])(=O)=O RSIJVJUOQBWMIM-UHFFFAOYSA-L 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229920001131 Pulp (paper) Polymers 0.000 description 1
- 239000007983 Tris buffer Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 210000003298 dental enamel Anatomy 0.000 description 1
- 239000002274 desiccant Substances 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 229940014144 folate Drugs 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229940126601 medicinal product Drugs 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- PHCBRBWANGJMHS-UHFFFAOYSA-J tetrasodium;disulfate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O PHCBRBWANGJMHS-UHFFFAOYSA-J 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
- C01D5/002—Preventing the absorption of moisture or caking of the crystals by additives
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention discloses hydrophobic superfine modified anhydrous sodium sulphate and a preparation method thereof. The invention can effectively improve the hydrophobic property of the hydrophobic superfine modified anhydrous sodium sulphate, effectively reduce the hygroscopic property of the anhydrous sodium sulphate, further effectively avoid the anhydrous sodium sulphate from generating moisture absorption, agglomeration and recrystallization in the production and processing process, and effectively ensure the service life of equipment; the dopamine hydrochloride surface contains a large number of hydroxyl functional groups, so that the active sites of condensation reaction can be effectively increased, and the subsequent structure formed on the surface of anhydrous sodium sulphate is more stable; after condensation reaction, introducing a long carbon chain of hexadecyl trimethoxy silane to the surface of anhydrous sodium sulphate, so that the surface contact angle of the anhydrous sodium sulphate is increased, and the surface of the anhydrous sodium sulphate is endowed with good hydrophobic property; the polydopamine coated folic acid is self-polymerized to form a micro-nano structure, so that the hydrophobic property of the anhydrous sodium sulphate is further improved.
Description
Technical Field
The invention relates to the technical field of anhydrous sodium sulphate, in particular to hydrophobic superfine modified anhydrous sodium sulphate and a preparation method thereof.
Background
The anhydrous sodium sulfate is generally sodium sulfate which is generated by combining sulfate radicals and sodium ionsSalt of the formula Na 2 SO 4 Sodium sulfate is soluble in water, and the solution is mostly neutral, soluble in glycerol and insoluble in ethanol. The high purity, finely divided sodium sulfate anhydrate is known as glauber's salt. The anhydrous sodium sulphate is easy to absorb water when exposed to the air, and generates sodium sulfate decahydrate, also known as mirabilite, which is slightly alkaline. It is mainly used for making water glass, enamel, paper pulp, glass, refrigerating mixing agent, drying agent, dye diluent, detergent, medicinal products, feed and analytical chemical reagent.
The existing superfine modified anhydrous sodium sulphate can corrode equipment after moisture absorption in the production process, and the service life of the equipment is seriously reduced.
Disclosure of Invention
In order to overcome the above-mentioned drawbacks of the prior art, embodiments of the present invention provide a hydrophobic type ultrafine modified anhydrous sodium sulphate and a preparation method thereof.
The hydrophobic superfine modified anhydrous sodium sulphate comprises the following components in percentage by weight: 2.6 to 3.6 percent of surfactant and the balance of anhydrous sodium sulphate.
Further, the surfactant comprises the following components in percentage by weight: 4.2-5.2% of hexadecyl trimethoxy silane, 0.08-0.12% of dopamine hydrochloride, 0.04-0.06% of folic acid, 0.10-0.14% of trihydroxymethyl aminomethane and the balance of absolute ethyl alcohol.
Further, the hydrophobic superfine modified anhydrous sodium sulphate comprises the following components in percentage by weight: 2.6 percent of surfactant and the balance of anhydrous sodium sulphate; the surfactant comprises the following components in percentage by weight: 4.2% of hexadecyl trimethoxy silane, 0.08% of dopamine hydrochloride, 0.04% of folic acid, 0.10% of trihydroxymethyl aminomethane and the balance of absolute ethyl alcohol.
Further, the hydrophobic superfine modified anhydrous sodium sulphate comprises the following components in percentage by weight: 3.6 percent of surfactant and the balance of anhydrous sodium sulphate; the surfactant comprises the following components in percentage by weight: 5.2 percent of hexadecyl trimethoxy silane, 0.12 percent of dopamine hydrochloride, 0.06 percent of folic acid, 0.14 percent of trihydroxymethyl aminomethane and the balance of absolute ethyl alcohol.
Further, the hydrophobic superfine modified anhydrous sodium sulphate comprises the following components in percentage by weight: 3.1 percent of surfactant and the balance of anhydrous sodium sulphate; the surfactant comprises the following components in percentage by weight: 4.7 percent of hexadecyl trimethoxy silane, 0.10 percent of dopamine hydrochloride, 0.05 percent of folic acid, 0.12 percent of trihydroxymethyl aminomethane and the balance of absolute ethyl alcohol.
The preparation method of the hydrophobic superfine modified anhydrous sodium sulphate comprises the following specific preparation steps:
the method comprises the following steps: weighing the anhydrous sodium sulphate, hexadecyl trimethoxy silane, dopamine hydrochloride, folic acid, trihydroxymethyl aminomethane and absolute ethyl alcohol in the surfactant raw materials in parts by weight;
step two: dropwise adding the hexadecyl trimethoxy silane in the step one into absolute ethyl alcohol at room temperature, and carrying out ultrasonic treatment for 10-20 minutes to obtain a mixed solution A;
step three: adding dopamine hydrochloride and folic acid in the first step into the mixed liquid A in the second step, carrying out water bath ultrasonic treatment for 10-20 minutes, carrying out water bath dark reaction for 16-20 hours, adding the tris (hydroxymethyl) aminomethane in the first step, and adjusting the pH value to 8-9 to obtain a surfactant;
step four: adding the anhydrous sodium sulphate obtained in the step one into a reactor, heating to 102-108 ℃, stirring, and exhausting for 10-20 minutes to obtain pretreated anhydrous sodium sulphate;
step five: spraying the surfactant in the fourth step into the anhydrous sodium sulphate pretreated in the fourth step through nitrogen, and stirring for 10-20 minutes to obtain hydrophobic modified anhydrous sodium sulphate;
step six: and D, adding the hydrophobic modified anhydrous sodium sulphate obtained in the step five into a pulverizer for grinding treatment to obtain the hydrophobic superfine modified anhydrous sodium sulphate.
Further, in the second step, the ultrasonic frequency is 1.4-1.6 MHz, and the ultrasonic power is 300-400W; in the third step, the water bath temperature is 50-70 ℃, the ultrasonic frequency is 40-60 KHz, and the ultrasonic power is 700-800W; in the fourth step, the stirring speed is 1200-1800 r/min; in the fifth step, the nitrogen conveying speed is 8-9 m/s, and the stirring rotating speed is 1050-1150 r/min; in the sixth step, the grinding speed is 1050-1150 r/min, and the particle size of the hydrophobic superfine modified anhydrous sodium sulphate is 1500-1900 meshes.
Further, in the second step, the ultrasonic frequency is 1.4MHz, and the ultrasonic power is 300W; in the third step, the temperature of the water bath is 50 ℃, the ultrasonic frequency is 40KHz, and the ultrasonic power is 700W; in the fourth step, the stirring speed is 1200 r/min; in the fifth step, the nitrogen conveying speed is 8m/s, and the stirring rotating speed is 1050 r/min; in the sixth step, the grinding speed is 1050r/min, and the granularity of the hydrophobic superfine modified anhydrous sodium sulphate is 1500 meshes.
Further, in the second step, the ultrasonic frequency is 1.6MHz, and the ultrasonic power is 400W; in the third step, the temperature of the water bath is 70 ℃, the ultrasonic frequency is 60KHz, and the ultrasonic power is 800W; in the fourth step, the stirring speed is 1800 r/min; in the fifth step, the nitrogen conveying speed is 9m/s, and the stirring rotating speed is 1150 r/min; in the sixth step, the grinding speed is 1150r/min, and the granularity of the hydrophobic superfine modified anhydrous sodium sulphate is 1900 meshes.
Further, in the second step, the ultrasonic frequency is 1.5MHz, and the ultrasonic power is 350W; in the third step, the water bath temperature is 60 ℃, the ultrasonic frequency is 50KHz, and the ultrasonic power is 750W; in the fourth step, the stirring speed is 1500 r/min; in the fifth step, the nitrogen conveying speed is 8.5m/s, and the stirring rotating speed is 1100 r/min; in the sixth step, the grinding speed is 1100r/min, and the granularity of the hydrophobic superfine modified anhydrous sodium sulphate is 1700 meshes.
The invention has the technical effects and advantages that:
1. the hydrophobic superfine modified anhydrous sodium sulphate prepared by the raw material formula can effectively improve the hydrophobic property of the hydrophobic superfine modified anhydrous sodium sulphate, effectively reduce the moisture absorption property of the anhydrous sodium sulphate, further effectively avoid the anhydrous sodium sulphate from generating excessive moisture absorption agglomeration recrystallization in the production and processing process, and effectively ensure the service life of equipment; hexadecyl trimethoxy silane in the surfactant is used as a silane coupling agent to perform hydrophobic modification treatment on the surface of the anhydrous sodium sulphate, so that the hydrophobic property of the anhydrous sodium sulphate can be effectively enhanced; the dopamine hydrochloride surface contains a large number of hydroxyl functional groups, so that the active sites of condensation reaction can be effectively increased, and the subsequent structure formed on the surface of anhydrous sodium sulphate is more stable; after condensation reaction, introducing a long carbon chain of hexadecyl trimethoxy silane to the surface of anhydrous sodium sulphate, so that the surface contact angle of the anhydrous sodium sulphate is increased, and the surface of the anhydrous sodium sulphate is endowed with good hydrophobic property; folic acid can jointly induce the polymerization of dopamine hydrochloride to form polydopamine through pi-pi interaction and hydrogen bonds; the polydopamine-coated folic acid is self-polymerized to form a micro-nano structure, hexadecyl trimethoxy silane is used for modifying a rough surface, and the hexadecyl trimethoxy silane and hydroxyl on the surface of modified anhydrous sodium sulphate are subjected to condensation reaction to improve the hydrophobicity of the anhydrous sodium sulphate and further improve the hydrophobic property of the anhydrous sodium sulphate;
2. in the process of preparing the hydrophobic superfine modified anhydrous sodium sulphate, hexadecyl trimethoxy silane is dripped into absolute ethyl alcohol, ultrasonic treatment is carried out for 10-20 minutes to obtain a mixed solution A, and the hexadecyl trimethoxy silane can be effectively dissolved and dispersed to form a silanol solution, so that the condensation reaction of subsequent silanol and hydroxyl of dopamine hydrochloride on the surface of the anhydrous sodium sulphate is facilitated, the long carbon chain of the hexadecyl trimethoxy silane is grafted to the surface of the anhydrous sodium sulphate, the hydrophobic treatment effect is further ensured, the anhydrous ethyl alcohol is used for dissolving, and the anhydrous sodium sulphate is prevented from absorbing moisture of water liquid when the anhydrous sodium sulphate is subjected to surface modification treatment subsequently; adding dopamine hydrochloride and folic acid into the mixed solution A, and after water bath ultrasonic treatment, performing water bath light-tight reaction, so that the dopamine hydrochloride and folic acid can be effectively guaranteed to perform composite reaction for self-polymerization; the trihydroxymethyl aminomethane is added to be used as a buffer solution, so that the stability of internal components can be effectively ensured; the anhydrous sodium sulphate is heated, stirred and exhausted, so that the anhydrous sodium sulphate can be effectively subjected to further cleaning and impurity removal treatment, and the moisture in the anhydrous sodium sulphate can be subjected to impurity removal treatment in the early stage; the surfactant is sprayed into the pretreated anhydrous sodium sulphate by taking nitrogen as carrier gas, so that the anhydrous sodium sulphate can be effectively and uniformly blown away, the surfactant is in contact with the surface of the anhydrous sodium sulphate under the rapid movement, the surfactant is fully reacted to carry out modification treatment on the surface of the anhydrous sodium sulphate, and the hydrophobic property of the anhydrous sodium sulphate can be effectively enhanced; grinding the hydrophobic modified anhydrous sodium sulphate to prepare the hydrophobic superfine modified anhydrous sodium sulphate.
Detailed Description
The following will clearly and completely describe the technical solutions in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
the invention provides hydrophobic superfine modified anhydrous sodium sulphate which comprises the following components in percentage by weight: 2.6 percent of surfactant and the balance of anhydrous sodium sulphate; the surfactant comprises the following components in percentage by weight: 4.2% of hexadecyl trimethoxy silane, 0.08% of dopamine hydrochloride, 0.04% of folic acid, 0.10% of trihydroxymethyl aminomethane and the balance of absolute ethyl alcohol;
anhydrous sodium sulfate was purchased from Shandong Zhi Jia chemical science and technology Co., Ltd, CAS number: 7757-82-6; hexadecyltrimethoxysilane was purchased from sigma aldrich trade ltd, CAS number: 16415-12-6, cargo number: v900620; dopamine hydrochloride was purchased from sigma aldrich (shanghai) trade ltd, CAS number: 62-31-7, cargo number: a PHR 1090; folate was purchased from shanghai yan chemical technology limited, CAS number: 59-30-3, cargo number: r010338; tris was purchased from shanghai yan chemical technology limited, CAS number: 77-86-1, cargo number: r052133; anhydrous ethanol was purchased from shanghai yan chemical technology limited, CAS No.: 64-17-5, cargo number: r033207;
the invention also provides a preparation method of the hydrophobic superfine modified anhydrous sodium sulphate, which comprises the following specific preparation steps:
the method comprises the following steps: weighing the anhydrous sodium sulphate, hexadecyl trimethoxy silane, dopamine hydrochloride, folic acid, trihydroxymethyl aminomethane and absolute ethyl alcohol in the surfactant raw materials in parts by weight;
step two: dropwise adding the hexadecyl trimethoxy silane in the step one into absolute ethyl alcohol at room temperature, and carrying out ultrasonic treatment for 10 minutes to obtain a mixed solution A;
step three: adding dopamine hydrochloride and folic acid in the first step into the mixed solution A in the second step, carrying out ultrasonic treatment in a water bath for 10 minutes, carrying out a water bath dark reaction for 16 hours, adding the tris (hydroxymethyl) aminomethane in the first step, and adjusting the pH value to 8 to obtain a surfactant;
step four: adding the anhydrous sodium sulphate obtained in the step one into a reactor, heating to 102 ℃, stirring and exhausting for 10 minutes to obtain pretreated anhydrous sodium sulphate;
step five: spraying the surfactant in the fourth step into the anhydrous sodium sulphate pretreated in the fourth step through nitrogen, and stirring for 10 minutes to obtain hydrophobic modified anhydrous sodium sulphate;
step six: and D, adding the hydrophobic modified anhydrous sodium sulphate obtained in the step five into a pulverizer for grinding treatment to obtain the hydrophobic superfine modified anhydrous sodium sulphate.
In the second step, the ultrasonic frequency is 1.4MHz, and the ultrasonic power is 300W; in the third step, the water bath temperature is 50 ℃, the ultrasonic frequency is 40KHz, and the ultrasonic power is 700W; in the fourth step, the stirring speed is 1200 r/min; in the fifth step, the nitrogen conveying speed is 8m/s, and the stirring rotating speed is 1050 r/min; in the sixth step, the grinding speed is 1050r/min, and the granularity of the hydrophobic superfine modified anhydrous sodium sulphate is 1500 meshes.
Example 2:
different from the embodiment 1, the hydrophobic superfine modified anhydrous sodium sulphate comprises the following components in percentage by weight: 3.6 percent of surfactant and the balance of anhydrous sodium sulphate; the surfactant comprises the following components in percentage by weight: 5.2 percent of hexadecyl trimethoxy silane, 0.12 percent of dopamine hydrochloride, 0.06 percent of folic acid, 0.14 percent of trihydroxymethyl aminomethane and the balance of absolute ethyl alcohol.
Example 3:
different from the examples 1-2, the hydrophobic superfine modified anhydrous sodium sulphate comprises the following components in percentage by weight: 3.1 percent of surfactant and the balance of anhydrous sodium sulphate; the surfactant comprises the following components in percentage by weight: 4.7 percent of hexadecyl trimethoxy silane, 0.10 percent of dopamine hydrochloride, 0.05 percent of folic acid, 0.12 percent of trihydroxymethyl aminomethane and the balance of absolute ethyl alcohol.
Example 4:
different from the embodiment 3, in the second step, the ultrasonic frequency is 1.6MHz, and the ultrasonic power is 400W; in the third step, the temperature of the water bath is 70 ℃, the ultrasonic frequency is 60KHz, and the ultrasonic power is 800W; in the fourth step, the stirring speed is 1800 r/min; in the fifth step, the nitrogen conveying speed is 9m/s, and the stirring rotating speed is 1150 r/min; in the sixth step, the grinding speed is 1150r/min, and the granularity of the hydrophobic superfine modified anhydrous sodium sulphate is 1900 meshes.
Example 5:
different from the embodiment 3, in the second step, the ultrasonic frequency is 1.5MHz, and the ultrasonic power is 350W; in the third step, the temperature of the water bath is 60 ℃, the ultrasonic frequency is 50KHz, and the ultrasonic power is 750W; in the fourth step, the stirring speed is 1500 r/min; in the fifth step, the nitrogen conveying speed is 8.5m/s, and the stirring rotating speed is 1100 r/min; in the sixth step, the grinding speed is 1100r/min, and the granularity of the hydrophobic superfine modified anhydrous sodium sulphate is 1700 meshes.
Example 6:
different from the embodiment 5, the preparation method of the hydrophobic superfine modified anhydrous sodium sulphate comprises the following specific preparation steps:
the method comprises the following steps: weighing the anhydrous sodium sulphate, hexadecyl trimethoxy silane, dopamine hydrochloride, folic acid, trihydroxymethyl aminomethane and absolute ethyl alcohol in the surfactant raw materials in parts by weight;
step two: dropwise adding the hexadecyl trimethoxy silane in the step one into absolute ethyl alcohol at room temperature, and carrying out ultrasonic treatment for 20 minutes to obtain a mixed solution A;
step three: adding dopamine hydrochloride and folic acid in the first step into the mixed solution A in the second step, carrying out ultrasonic treatment in a water bath for 20 minutes, carrying out a reaction in a water bath in a dark place for 20 hours, adding the tris (hydroxymethyl) aminomethane in the first step, and adjusting the pH value to 9 to obtain a surfactant;
step four: adding the anhydrous sodium sulphate obtained in the step one into a reactor, heating to 108 ℃, stirring and exhausting for 20 minutes to obtain pretreated anhydrous sodium sulphate;
step five: spraying the surfactant in the fourth step into the anhydrous sodium sulphate pretreated in the fourth step through nitrogen, and stirring for 20 minutes at the same time to obtain hydrophobic modified anhydrous sodium sulphate;
step six: and D, adding the hydrophobic modified anhydrous sodium sulphate obtained in the step five into a pulverizer for grinding treatment to obtain the hydrophobic superfine modified anhydrous sodium sulphate.
Example 7:
different from the embodiment 5, the preparation method of the hydrophobic superfine modified anhydrous sodium sulphate comprises the following specific preparation steps:
the method comprises the following steps: weighing the anhydrous sodium sulphate, hexadecyl trimethoxy silane, dopamine hydrochloride, folic acid, trihydroxymethyl aminomethane and absolute ethyl alcohol in the surfactant raw materials in parts by weight;
step two: dropwise adding the hexadecyl trimethoxy silane in the step one into absolute ethyl alcohol at room temperature, and carrying out ultrasonic treatment for 15 minutes to obtain a mixed solution A;
step three: adding dopamine hydrochloride and folic acid in the first step into the mixed solution A in the second step, carrying out ultrasonic treatment in a water bath for 15 minutes, carrying out a water bath dark reaction for 18 hours, adding the tris (hydroxymethyl) aminomethane in the first step, and adjusting the pH value to 8.5 to obtain a surfactant;
step four: adding the anhydrous sodium sulphate obtained in the step one into a reactor, heating to 105 ℃, stirring and exhausting for 15 minutes to obtain pretreated anhydrous sodium sulphate;
step five: spraying the surfactant in the fourth step into the anhydrous sodium sulphate pretreated in the fourth step through nitrogen, and stirring for 15 minutes to obtain hydrophobic modified anhydrous sodium sulphate;
step six: and D, adding the hydrophobic modified anhydrous sodium sulphate obtained in the step five into a pulverizer for grinding treatment to obtain the hydrophobic superfine modified anhydrous sodium sulphate.
Comparative example 1:
the difference from example 3 is: the hydrophobic superfine modified anhydrous sodium sulphate comprises the following components in percentage by weight: 3.1 percent of surfactant and the balance of anhydrous sodium sulphate; the surfactant comprises the following components in percentage by weight: 0.10% of dopamine hydrochloride, 0.05% of folic acid, 0.12% of tris (hydroxymethyl) aminomethane and the balance of absolute ethyl alcohol.
Comparative example 2:
the difference from example 3 is: the hydrophobic superfine modified anhydrous sodium sulphate comprises the following components in percentage by weight: 3.1 percent of surfactant and the balance of anhydrous sodium sulphate; the surfactant comprises the following components in percentage by weight: 4.7 percent of hexadecyl trimethoxy silane, 0.05 percent of folic acid, 0.12 percent of trihydroxymethyl aminomethane and the balance of absolute ethyl alcohol.
Comparative example 3:
the differences from example 3 are: the hydrophobic superfine modified anhydrous sodium sulphate comprises the following components in percentage by weight: 3.1 percent of surfactant and the balance of anhydrous sodium sulphate; the surfactant comprises the following components in percentage by weight: 4.7 percent of hexadecyl trimethoxy silane, 0.10 percent of dopamine hydrochloride, 0.12 percent of tris (hydroxymethyl) aminomethane and the balance of absolute ethyl alcohol.
Comparative example 4:
the difference from example 7 is: directly blending the raw materials of the surfactant to prepare the surfactant.
Comparative example 5:
the difference from example 7 is: in step five, the surfactant is directly added into the pretreated anhydrous sodium sulphate for blending.
The hydrophobic superfine modified anhydrous sodium sulfate produced in the examples and the comparative examples is detected, and the moisture absorption rates of the pretreated anhydrous sodium sulfate and the hydrophobic superfine modified anhydrous sodium sulfate are detected according to the GB/T169913-2008 standard; the results obtained are shown in the following table:
from the above table, it can be seen that: the invention can effectively improve the hydrophobic property of the hydrophobic superfine modified anhydrous sodium sulphate, effectively reduce the hygroscopic property of the anhydrous sodium sulphate, further effectively avoid the excessive hygroscopic agglomeration and recrystallization of the anhydrous sodium sulphate in the production and processing process, and effectively ensure the service life of equipment.
According to the invention, hexadecyl trimethoxy silane in the surfactant is used as a silane coupling agent to perform hydrophobic modification treatment on the surface of anhydrous sodium sulphate, so that the hydrophobic property of the anhydrous sodium sulphate can be effectively enhanced; the dopamine hydrochloride surface contains a large number of hydroxyl functional groups, so that the active sites of condensation reaction can be effectively increased, and the subsequent structure formed on the surface of anhydrous sodium sulphate is more stable; after condensation reaction, introducing a long carbon chain of hexadecyl trimethoxy silane to the surface of the anhydrous sodium sulphate, so that the surface contact angle of the anhydrous sodium sulphate is increased, and the surface of the anhydrous sodium sulphate is endowed with good hydrophobic property; folic acid can jointly induce the polymerization of dopamine hydrochloride to form polydopamine through pi-pi interaction and hydrogen bonds; the polydopamine-coated folic acid is self-polymerized to form a micro-nano structure, hexadecyl trimethoxy silane is used for modifying a rough surface, and the hexadecyl trimethoxy silane and hydroxyl on the surface of modified anhydrous sodium sulphate are subjected to condensation reaction to improve the hydrophobicity of the anhydrous sodium sulphate and further improve the hydrophobic property of the anhydrous sodium sulphate; in the second step, hexadecyl trimethoxy silane is dripped into absolute ethyl alcohol, ultrasonic treatment is carried out for 10-20 minutes to obtain a mixed solution A, the hexadecyl trimethoxy silane can be effectively dissolved and dispersed to form a silanol solution, subsequent condensation reaction of silanol and hydroxyl of dopamine hydrochloride on the surface of anhydrous sodium sulphate is facilitated, then long carbon chains of the hexadecyl trimethoxy silane are grafted to the surface of the anhydrous sodium sulphate, the hydrophobic treatment effect is further ensured, the absolute ethyl alcohol is used for dissolving, and the anhydrous sodium sulphate is prevented from absorbing moisture of water liquid when the anhydrous sodium sulphate is subjected to surface modification treatment subsequently; in the third step, dopamine hydrochloride and folic acid are added into the mixed solution A, and after water bath ultrasonic treatment, water bath light-resistant reaction is carried out, so that the dopamine hydrochloride and folic acid can be effectively guaranteed to carry out composite reaction for self-polymerization; the trihydroxymethyl aminomethane is added to be used as a buffer solution, so that the stability of internal components can be effectively ensured; in the fourth step, the anhydrous sodium sulphate is subjected to heating, stirring and exhaust treatment, so that the anhydrous sodium sulphate can be effectively further cleaned and subjected to impurity removal treatment, and the moisture in the anhydrous sodium sulphate can be subjected to impurity removal treatment in the early stage; in the fifth step, the surfactant is sprayed into the pretreated anhydrous sodium sulphate by taking nitrogen as carrier gas, so that the anhydrous sodium sulphate can be effectively and uniformly blown away, the surfactant is in contact with the surface of the anhydrous sodium sulphate under the rapid movement, the surfactant is fully reacted to carry out modification treatment on the surface of the anhydrous sodium sulphate, and the hydrophobic property of the anhydrous sodium sulphate can be effectively enhanced; and step six, grinding the hydrophobically modified anhydrous sodium sulphate to prepare the hydrophobic superfine modified anhydrous sodium sulphate.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The hydrophobic superfine modified anhydrous sodium sulphate is characterized in that: comprises the following components in percentage by weight: 2.6 to 3.6 percent of surfactant and the balance of anhydrous sodium sulphate.
2. The hydrophobic ultrafine modified anhydrous sodium sulphate according to claim 1, characterized in that: the surfactant comprises the following components in percentage by weight: 4.2-5.2% of hexadecyl trimethoxy silane, 0.08-0.12% of dopamine hydrochloride, 0.04-0.06% of folic acid, 0.10-0.14% of trihydroxymethyl aminomethane and the balance of absolute ethyl alcohol.
3. The hydrophobic ultrafine modified anhydrous sodium sulphate according to claim 2, characterized in that: comprises the following components in percentage by weight: 2.6 percent of surfactant and the balance of anhydrous sodium sulphate; the surfactant comprises the following components in percentage by weight: 4.2% of hexadecyl trimethoxy silane, 0.08% of dopamine hydrochloride, 0.04% of folic acid, 0.10% of trihydroxymethyl aminomethane and the balance of absolute ethyl alcohol.
4. The hydrophobic ultrafine modified anhydrous sodium sulphate according to claim 2, characterized in that: comprises the following components in percentage by weight: 3.6 percent of surfactant and the balance of anhydrous sodium sulphate; the surfactant comprises the following components in percentage by weight: 5.2 percent of hexadecyl trimethoxy silane, 0.12 percent of dopamine hydrochloride, 0.06 percent of folic acid, 0.14 percent of trihydroxymethyl aminomethane and the balance of absolute ethyl alcohol.
5. The hydrophobic ultrafine modified anhydrous sodium sulfate according to claim 2, wherein: comprises the following components in percentage by weight: 3.1 percent of surfactant and the balance of anhydrous sodium sulphate; the surfactant comprises the following components in percentage by weight: 4.7 percent of hexadecyl trimethoxy silane, 0.10 percent of dopamine hydrochloride, 0.05 percent of folic acid, 0.12 percent of trihydroxymethyl aminomethane and the balance of absolute ethyl alcohol.
6. The preparation method of the hydrophobic superfine modified anhydrous sodium sulphate is characterized by comprising the following steps: the preparation method comprises the following specific steps:
the method comprises the following steps: weighing the anhydrous sodium sulphate, hexadecyl trimethoxy silane, dopamine hydrochloride, folic acid, trihydroxymethyl aminomethane and absolute ethyl alcohol in the surfactant raw materials in parts by weight;
step two: dropwise adding the hexadecyl trimethoxy silane in the first step into absolute ethyl alcohol at room temperature, and carrying out ultrasonic treatment for 10-20 minutes to obtain a mixed solution A;
step three: adding dopamine hydrochloride and folic acid in the first step into the mixed liquid A in the second step, carrying out water bath ultrasonic treatment for 10-20 minutes, carrying out water bath dark reaction for 16-20 hours, adding the tris (hydroxymethyl) aminomethane in the first step, and adjusting the pH value to 8-9 to obtain a surfactant;
step four: adding the anhydrous sodium sulphate obtained in the step one into a reactor, heating to 102-108 ℃, stirring, and exhausting for 10-20 minutes to obtain pretreated anhydrous sodium sulphate;
step five: spraying the surfactant in the fourth step into the anhydrous sodium sulphate pretreated in the fourth step through nitrogen, and stirring for 10-20 minutes to obtain hydrophobic modified anhydrous sodium sulphate;
step six: and D, adding the hydrophobic modified anhydrous sodium sulphate obtained in the step five into a pulverizer for grinding treatment to obtain the hydrophobic superfine modified anhydrous sodium sulphate.
7. The method for preparing the hydrophobic superfine modified anhydrous sodium sulphate according to claim 6, which is characterized in that: in the second step, the ultrasonic frequency is 1.4-1.6 MHz, and the ultrasonic power is 300-400W; in the third step, the water bath temperature is 50-70 ℃, the ultrasonic frequency is 40-60 KHz, and the ultrasonic power is 700-800W; in the fourth step, the stirring speed is 1200-1800 r/min; in the fifth step, the nitrogen conveying speed is 8-9 m/s, and the stirring rotating speed is 1050-1150 r/min; in the sixth step, the grinding rotation speed is 1050-1150 r/min, and the particle size of the hydrophobic superfine modified anhydrous sodium sulphate is 1500-1900 meshes.
8. The method for preparing the hydrophobic superfine modified anhydrous sodium sulphate according to claim 7, which is characterized in that: in the second step, the ultrasonic frequency is 1.4MHz, and the ultrasonic power is 300W; in the third step, the temperature of the water bath is 50 ℃, the ultrasonic frequency is 40KHz, and the ultrasonic power is 700W; in the fourth step, the stirring speed is 1200 r/min; in the fifth step, the nitrogen conveying speed is 8m/s, and the stirring rotating speed is 1050 r/min; in the sixth step, the grinding speed is 1050r/min, and the granularity of the hydrophobic superfine modified anhydrous sodium sulphate is 1500 meshes.
9. The method for preparing the hydrophobic superfine modified anhydrous sodium sulphate according to claim 7, which is characterized in that: in the second step, the ultrasonic frequency is 1.6MHz, and the ultrasonic power is 400W; in the third step, the water bath temperature is 70 ℃, the ultrasonic frequency is 60KHz, and the ultrasonic power is 800W; in the fourth step, the stirring speed is 1800 r/min; in the fifth step, the nitrogen conveying speed is 9m/s, and the stirring rotating speed is 1150 r/min; in the sixth step, the grinding speed is 1150r/min, and the granularity of the hydrophobic superfine modified anhydrous sodium sulphate is 1900 meshes.
10. The method for preparing the hydrophobic superfine modified anhydrous sodium sulphate according to claim 7, which is characterized in that: in the second step, the ultrasonic frequency is 1.5MHz, and the ultrasonic power is 350W; in the third step, the temperature of the water bath is 60 ℃, the ultrasonic frequency is 50KHz, and the ultrasonic power is 750W; in the fourth step, the stirring speed is 1500 r/min; in the fifth step, the nitrogen conveying speed is 8.5m/s, and the stirring rotating speed is 1100 r/min; in the sixth step, the grinding speed is 1100r/min, and the granularity of the hydrophobic superfine modified anhydrous sodium sulphate is 1700 meshes.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102516818A (en) * | 2011-11-16 | 2012-06-27 | 和昌（广西）化工有限公司 | Production method for superfine modified anhydrous sodium sulphate |
| CN104831534A (en) * | 2015-03-06 | 2015-08-12 | 哈尔滨工业大学宜兴环保研究院 | Super-hydrophobic and -oleophylic cloth producing method |
| CN112538762A (en) * | 2020-12-16 | 2021-03-23 | 江苏理工学院 | Method for preparing stable super-hydrophobic antibacterial fabric by one-pot method |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102516818A (en) * | 2011-11-16 | 2012-06-27 | 和昌（广西）化工有限公司 | Production method for superfine modified anhydrous sodium sulphate |
| CN104831534A (en) * | 2015-03-06 | 2015-08-12 | 哈尔滨工业大学宜兴环保研究院 | Super-hydrophobic and -oleophylic cloth producing method |
| CN112538762A (en) * | 2020-12-16 | 2021-03-23 | 江苏理工学院 | Method for preparing stable super-hydrophobic antibacterial fabric by one-pot method |
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