CN116715501B - Antistatic calcium sulfate floor substrate and preparation method thereof - Google Patents
Antistatic calcium sulfate floor substrate and preparation method thereof Download PDFInfo
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- CN116715501B CN116715501B CN202310987235.3A CN202310987235A CN116715501B CN 116715501 B CN116715501 B CN 116715501B CN 202310987235 A CN202310987235 A CN 202310987235A CN 116715501 B CN116715501 B CN 116715501B
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- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 title claims abstract description 88
- 239000000758 substrate Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 44
- 229920000858 Cyclodextrin Polymers 0.000 claims abstract description 36
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 33
- 238000003756 stirring Methods 0.000 claims abstract description 31
- 239000000843 powder Substances 0.000 claims abstract description 30
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 24
- 150000001412 amines Chemical class 0.000 claims abstract description 23
- -1 sulfhydryl cyclodextrin Chemical compound 0.000 claims abstract description 23
- 238000001035 drying Methods 0.000 claims abstract description 22
- 239000000463 material Substances 0.000 claims abstract description 20
- 239000002994 raw material Substances 0.000 claims abstract description 20
- 238000005096 rolling process Methods 0.000 claims abstract description 19
- BCAARMUWIRURQS-UHFFFAOYSA-N dicalcium;oxocalcium;silicate Chemical compound [Ca+2].[Ca+2].[Ca]=O.[O-][Si]([O-])([O-])[O-] BCAARMUWIRURQS-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000003822 epoxy resin Substances 0.000 claims abstract description 18
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 18
- 229910021534 tricalcium silicate Inorganic materials 0.000 claims abstract description 18
- 235000019976 tricalcium silicate Nutrition 0.000 claims abstract description 18
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 14
- 239000004917 carbon fiber Substances 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 14
- 229920001131 Pulp (paper) Polymers 0.000 claims abstract description 12
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 12
- ZOMBKNNSYQHRCA-UHFFFAOYSA-J calcium sulfate hemihydrate Chemical compound O.[Ca+2].[Ca+2].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O ZOMBKNNSYQHRCA-UHFFFAOYSA-J 0.000 claims abstract description 11
- 239000010451 perlite Substances 0.000 claims abstract description 10
- 235000019362 perlite Nutrition 0.000 claims abstract description 10
- SHFGJEQAOUMGJM-UHFFFAOYSA-N dialuminum dipotassium disodium dioxosilane iron(3+) oxocalcium oxomagnesium oxygen(2-) Chemical compound [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[Na+].[Na+].[Al+3].[Al+3].[K+].[K+].[Fe+3].[Fe+3].O=[Mg].O=[Ca].O=[Si]=O SHFGJEQAOUMGJM-UHFFFAOYSA-N 0.000 claims abstract description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 30
- ICSNLGPSRYBMBD-UHFFFAOYSA-N 2-aminopyridine Chemical compound NC1=CC=CC=N1 ICSNLGPSRYBMBD-UHFFFAOYSA-N 0.000 claims description 17
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 13
- BCMYXYHEMGPZJN-UHFFFAOYSA-N 1-chloro-2-isocyanatoethane Chemical compound ClCCN=C=O BCMYXYHEMGPZJN-UHFFFAOYSA-N 0.000 claims description 12
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- QIOYHIUHPGORLS-UHFFFAOYSA-N n,n-dimethyl-3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN(C)C QIOYHIUHPGORLS-UHFFFAOYSA-N 0.000 claims description 12
- HFHDHCJBZVLPGP-UHFFFAOYSA-N schardinger α-dextrin Chemical compound O1C(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(O)C2O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC2C(O)C(O)C1OC2CO HFHDHCJBZVLPGP-UHFFFAOYSA-N 0.000 claims description 11
- XUJNEKJLAYXESH-REOHCLBHSA-N L-Cysteine Chemical compound SC[C@H](N)C(O)=O XUJNEKJLAYXESH-REOHCLBHSA-N 0.000 claims description 9
- XUJNEKJLAYXESH-UHFFFAOYSA-N cysteine Natural products SCC(N)C(O)=O XUJNEKJLAYXESH-UHFFFAOYSA-N 0.000 claims description 9
- 235000018417 cysteine Nutrition 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 8
- 229920005646 polycarboxylate Polymers 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 8
- BRLQWZUYTZBJKN-UHFFFAOYSA-N Epichlorohydrin Chemical compound ClCC1CO1 BRLQWZUYTZBJKN-UHFFFAOYSA-N 0.000 claims description 6
- JMFJXZKGJLFGEJ-UHFFFAOYSA-N isocyanic acid;pyridine Chemical compound N=C=O.C1=CC=NC=C1 JMFJXZKGJLFGEJ-UHFFFAOYSA-N 0.000 claims description 6
- MYWOJODOMFBVCB-UHFFFAOYSA-N 1,2,6-trimethylphenanthrene Chemical compound CC1=CC=C2C3=CC(C)=CC=C3C=CC2=C1C MYWOJODOMFBVCB-UHFFFAOYSA-N 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 5
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 238000004821 distillation Methods 0.000 claims description 3
- 125000001624 naphthyl group Chemical group 0.000 claims description 3
- LRWZZZWJMFNZIK-UHFFFAOYSA-N 2-chloro-3-methyloxirane Chemical compound CC1OC1Cl LRWZZZWJMFNZIK-UHFFFAOYSA-N 0.000 claims description 2
- 238000006703 hydration reaction Methods 0.000 abstract description 16
- 230000036571 hydration Effects 0.000 abstract description 15
- 230000002708 enhancing effect Effects 0.000 abstract description 2
- 238000007711 solidification Methods 0.000 abstract description 2
- 230000008023 solidification Effects 0.000 abstract description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 12
- 239000000835 fiber Substances 0.000 description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 6
- 230000006835 compression Effects 0.000 description 4
- 238000007906 compression Methods 0.000 description 4
- 239000012948 isocyanate Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- WHGYBXFWUBPSRW-FOUAGVGXSA-N beta-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO WHGYBXFWUBPSRW-FOUAGVGXSA-N 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- DGVVJWXRCWCCOD-UHFFFAOYSA-N naphthalene;hydrate Chemical compound O.C1=CC=CC2=CC=CC=C21 DGVVJWXRCWCCOD-UHFFFAOYSA-N 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 150000003242 quaternary ammonium salts Chemical group 0.000 description 3
- 229920006395 saturated elastomer Polymers 0.000 description 3
- 125000003396 thiol group Chemical group [H]S* 0.000 description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- 239000001116 FEMA 4028 Substances 0.000 description 2
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 235000011175 beta-cyclodextrine Nutrition 0.000 description 2
- 229960004853 betadex Drugs 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- CUIGSPBMMQWNLR-UHFFFAOYSA-N 2-isocyanatopyridine Chemical compound O=C=NC1=CC=CC=N1 CUIGSPBMMQWNLR-UHFFFAOYSA-N 0.000 description 1
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 1
- 229910001335 Galvanized steel Inorganic materials 0.000 description 1
- 229920000877 Melamine resin Polymers 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- KNSXNCFKSZZHEA-UHFFFAOYSA-N [3-prop-2-enoyloxy-2,2-bis(prop-2-enoyloxymethyl)propyl] prop-2-enoate Chemical compound C=CC(=O)OCC(COC(=O)C=C)(COC(=O)C=C)COC(=O)C=C KNSXNCFKSZZHEA-UHFFFAOYSA-N 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 150000003927 aminopyridines Chemical class 0.000 description 1
- 230000003712 anti-aging effect Effects 0.000 description 1
- 239000002216 antistatic agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910001424 calcium ion Inorganic materials 0.000 description 1
- ZHZFKLKREFECML-UHFFFAOYSA-L calcium;sulfate;hydrate Chemical compound O.[Ca+2].[O-]S([O-])(=O)=O ZHZFKLKREFECML-UHFFFAOYSA-L 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000001934 delay Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000008397 galvanized steel Substances 0.000 description 1
- 239000010440 gypsum Substances 0.000 description 1
- 229910052602 gypsum Inorganic materials 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 235000012054 meals Nutrition 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 1
- FWFGVMYFCODZRD-UHFFFAOYSA-N oxidanium;hydrogen sulfate Chemical compound O.OS(O)(=O)=O FWFGVMYFCODZRD-UHFFFAOYSA-N 0.000 description 1
- 239000010893 paper waste Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 238000005956 quaternization reaction Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 230000000979 retarding effect Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 150000003512 tertiary amines Chemical class 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
-
- 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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
Landscapes
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The application relates to the field of calcium sulfate floors, in particular to an antistatic calcium sulfate floor base material and a preparation method thereof. The preparation process comprises the following steps: step 1: mixing and stirring calcium sulfate hemihydrate, tricalcium silicate, perlite and chopped carbon fiber to obtain powder; step 2: preparing sulfhydryl cyclodextrin; step 3: sequentially adding sulfhydryl cyclodextrin and amine curing agent into paper pulp, and uniformly mixing; adding powder and a water reducing agent, and stirring and mixing; adding the aqueous epoxy resin and the curing accelerator, and stirring and mixing to obtain a substrate raw material; step 4: pouring the substrate raw material into a mould, and rolling and forming; steam curing and drying; to obtain the antistatic calcium sulfate floor base material. In the scheme, an inorganic network is formed by powder hydration, and an organic network is formed by epoxy resin solidification; the inorganic network and the organic network form an interpenetrating network, thereby effectively improving the compactness of the calcium sulfate floor and enhancing the mechanical strength.
Description
Technical Field
The application relates to the technical field of calcium sulfate floors, in particular to an antistatic calcium sulfate floor base material and a preparation method thereof.
Background
The antistatic calcium sulfate floor is a special floor which can effectively prevent static electricity, is environment-friendly, fireproof and high in safety. The device is commonly used in places sensitive to static electricity such as computer rooms, power dispatching rooms, purifying factories, electronic production rooms, chemical laboratories, hospitals and the like, and relates to a plurality of fields such as telecommunication, power, electronics, chemical industry, medical treatment and the like, and the device is widely applied.
The antistatic calcium sulfate floor is generally prepared by stacking a steel plate bottom surface, a calcium sulfate floor base material and an antistatic veneer. The main material of the calcium sulfate floor base material is calcium sulfate, and compared with a cement material, the calcium sulfate floor base material has lower density, large pores and lower mechanical strength; and fiber pulp is generally added, while water saturated fibers affect the hydration of calcium sulfate, reducing the overall strength of the substrate. On the other hand, in order to enhance the antistatic performance, an antistatic material is introduced, and firstly, the problem of uniform dispersibility exists, and secondly, more materials are required to be added to form an antistatic network.
In summary, the problems are solved, and the preparation of the calcium sulfate floor substrate with high mechanical strength and good antistatic performance has important application significance.
Disclosure of Invention
The application aims to provide an antistatic calcium sulfate floor substrate and a preparation method thereof, which are used for solving the problems in the background technology.
In order to solve the technical problems, the application provides the following technical scheme:
the preparation method of the antistatic calcium sulfate floor base material comprises the following steps:
step 1: mixing and stirring calcium sulfate hemihydrate, tricalcium silicate, perlite and chopped carbon fiber to obtain powder;
step 2: adding cyclodextrin into water, adding potassium hydroxide, and stirring for dissolving; adding 2-aminopyridine and cysteine at 50-55 ℃; at 60-65 ℃, epoxy chloropropane is added dropwise for reaction for 1-2 hours; adjusting the pH to be 5-6, adding absolute ethyl alcohol, standing, filtering, purifying and drying to obtain sulfhydryl cyclodextrin;
step 3: sequentially adding sulfhydryl cyclodextrin and amine curing agent into paper pulp, and uniformly mixing; adding powder and a water reducing agent, and stirring and mixing; adding the aqueous epoxy resin and the curing accelerator, and stirring and mixing to obtain a substrate raw material;
step 4: pouring the substrate raw material into a mould, and rolling and forming; steam curing and drying; to obtain the antistatic calcium sulfate floor base material.
Wherein, the sulfhydryl cyclodextrin is prepared by grafting cysteine and aminopyridine on cyclodextrin by using epichlorohydrin as linking, utilizing the reaction of chlorine and hydroxyl and the reaction of epoxy group and amino. The sulfhydryl cyclodextrin has carboxyl and sulfhydryl groups, delays hydration reaction between calcium ions and sulfate ions and water, has retarding property, can improve hydration process and strength. And the sulfhydryl contained in the epoxy resin can cure the epoxy resin at low temperature, and the carboxyl can cure the epoxy resin at higher temperature, so that different curing mechanisms are generated, and the curing stress is reduced. In addition, the grafted pyridine effectively enhances the antistatic effect.
More preferably, the substrate material comprises the following components: 100 parts of powder, 76-80 parts of paper pulp, 0.4-0.8 part of water reducer, 7.5-12.5 parts of water-based epoxy resin, 2.3-2.8 parts of amine curing agent, 1.2-1.8 parts of sulfhydryl cyclodextrin and 0.2-0.3 part of curing accelerator.
More preferably, the raw materials of the sulfhydryl cyclodextrin comprise the following components: the anti-aging agent comprises, by weight, 10 parts of cyclodextrin, 2.5-3.5 parts of 2-aminopyridine, 11-13 parts of cysteine and 13-15 parts of epichlorohydrin.
More preferably, the powder comprises the following components: 65-75 parts of calcium sulfate hemihydrate, 13-15 parts of tricalcium silicate, 10-16 parts of perlite and 2-4 parts of chopped carbon fiber.
Wherein, tricalcium silicate is introduced into the powder, and the hydration rate of the whole powder is reduced by utilizing the property of low hydration rate. Thereby improving the hydration influence of water saturated fiber in the paper pulp on the gel in advance existing in the powder. In addition, as the hydration rate of the tricalcium silicate is slower than that of the calcium sulfate hemihydrate, hydration products of the tricalcium silicate can be filled in gaps of calcium sulfate hydrate, so that the compactness is improved; the mechanical strength is enhanced.
The chopped carbon fiber is introduced into the powder, one of the chopped carbon fiber is an inorganic network generated by reinforcing the powder, and the other of the chopped carbon fiber can form an antistatic network with quaternary ammonium salt groups, pyridine groups and the like existing in an organic network generated by curing epoxy resin, so that the antistatic performance of the calcium sulfate floor substrate is effectively enhanced.
More preferably, the pulp is industrial pulp with the weight of 5-8wt%.
Wherein, the fiber contained in the paper pulp can enhance the toughness and strength of the calcium sulfate floor; however, the fiber is not easy to be excessively introduced, firstly, the water supersaturated fiber is more introduced, and the hydration process is influenced; secondly, entanglement of the fibers causes problems of dispersibility, resulting in a decrease in strength. In addition, in order to improve the influence of pulp on hydration, early hydration is inhibited by introducing tricalcium silicate, a combination water reducing agent, and mercapto cyclodextrin into the raw material.
More optimally, the water reducer consists of a polycarboxylate water reducer and a naphthalene-based water reducer in a mass ratio of 5:3.
The polycarboxylate water reducer can effectively slow down the whole hydration process, the naphthyl water reducer strengthens the later-stage speed reduction, and the two components are matched, so that a denser inorganic network can be realized.
More optimally, the roll forming process is as follows: rolling for 20-30 minutes at room temperature under 1-2 mpa, and rolling for 20-30 minutes at 80-100 ℃ under 5-8 mpa; rolling for 10-15 minutes at 120-140 ℃ and 10-12 mpa; the steam curing time is 3-5 hours; the drying conditions are as follows: and drying at 60-100 ℃ for 20-30 hours.
More optimally, the preparation method of the amine curing agent comprises the following steps: (1) Sequentially adding ethylenediamine and pentaerythritol tetraacrylate into methanol, reacting for 20-24 hours at 50-55 ℃, and performing reduced pressure distillation, washing and drying to obtain a polyamino tree-like product; (2) Adding the polyamino tree-like product into toluene, adding 2-chloroethyl isocyanate and isocyanate pyridine at 0-5 ℃, and stirring for 10-12 hours; adding (N, N-dimethyl-3-aminopropyl) trimethoxysilane, N-dimethylacetamide and toluene, stirring for 2-3 days at 80-85 ℃, purifying and drying to obtain the amine curing agent.
Wherein the polyamino tree-like product is a product with four arms, which is prepared by taking ethylenediamine and pentaerythritol tetraacrylate as reaction; which can cure the epoxy resin directly.
Furthermore, in order to enhance the antistatic property and the mechanical strength of the calcium sulfate floor base material, the polyamino tree-like product is modified to prepare the amine curing agent. The modification process is that firstly, the terminal amino group of the polyamino tree-shaped product reacts with isocyanate groups, and 2-chloroethyl isocyanate and isocyanate pyridine are partially grafted; and then the chlorine of the 2-chloroethyl isocyanate and tertiary amine in the (N, N-dimethyl-3-aminopropyl) trimethoxy silane are utilized to generate quaternization reaction.
Wherein, the grafting of isocyanate pyridine increases the compatibility with sulfhydryl cyclodextrin and increases antistatic property; the grafting of the 2-chloroethyl isocyanate is connected with the grafting of the (N, N-dimethyl-3-aminopropyl) trimethoxysilane, and the generated quaternary ammonium salt group can improve the antistatic performance, and the (N, N-dimethyl-3-aminopropyl) trimethoxysilane can improve the fluidity of the amine curing agent in powder, and improve the uniform dispersion of the powder. Meanwhile, the amine curing agent is a four-arm product, so that the toughness and bending performance of the calcium sulfate floor base material can be enhanced.
More optimally, in the raw materials of the polyamino tree-shaped product, the raw materials of the amine curing agent comprise, by weight, 10 parts of the polyamino tree-shaped product, 1.4-1.6 parts of 2-chloroethyl isocyanate, 1.5-1.8 parts of isocyanate pyridine and 3.2-3.5 parts of (N, N-dimethyl-3-aminopropyl) trimethoxysilane.
More optimally, the antistatic calcium sulfate floor substrate is prepared by the preparation method of the antistatic calcium sulfate floor substrate.
Compared with the prior art, the application has the beneficial effects that:
(1) Forming an inorganic network through powder hydration, and forming an organic network through epoxy resin solidification; the inorganic network and the organic network form an interpenetrating network, thereby effectively improving the compactness of the calcium sulfate floor and enhancing the mechanical strength.
(2) By introducing the tricalcium silicate, the combined water reducing agent and the sulfhydryl cyclodextrin, the influence of water saturated fibers in paper pulp on powder hydration is inhibited, the hydration process is effectively improved, the compactness of an inorganic network is enhanced, and the mechanical strength of a calcium sulfate floor substrate is enhanced.
(3) By introducing sulfhydryl cyclodextrin and amine curing agent and utilizing the curing process of different groups, the curing stress of the epoxy resin is effectively reduced, and the shrinkage is reduced, so that the mechanical strength of the calcium sulfate floor substrate is improved; meanwhile, the groups such as pyridine and quaternary ammonium salt are used to form an antistatic network with the chopped carbon fibers in the powder, so that the antistatic performance of the calcium sulfate floor base material is enhanced.
Detailed Description
The following description of the technical solutions in the embodiments of the present application will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present application, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application.
It should be noted that the manufacturers of all the raw materials according to the present application include, without any particular limitation: in the following examples, calcium sulfate hemihydrate was 95% pure and was obtained from Shandong Tongbang gypsum product Co., ltd, ground and sieved through a 100 mesh sieve for use; the purity of the tricalcium silicate is 95%, the tricalcium silicate is obtained from Shandong national chemical Co., ltd, and the tricalcium silicate is ground and sieved by a 150-mesh sieve for use; the density of the perlite is 2.4g/cm 3 The granularity is 80 meshes, and the powder is from Yongkai heat-insulating material Co., ltd; chopped carbon fibers with the diameter of 5-10 mu m are sourced from Shanghai composite material science and technology Co., ltd; the model of the polycarboxylate water reducer is SP-409, and the model of the naphthyl water reducer is SSF-1000; the cyclodextrin is beta-cyclodextrin, the CAS number is 7585-39-9, and the cyclodextrin is from Zhengzhou alpha chemical company; the model of the water-based epoxy resin is WG827, and is derived from Shandong Jiayi chemical technology Co., ltd; pentaerythritol tetraacrylate has a CAS number of 4986-89-4, 2-chloroethyl isocyanate of 1943-83-5, (N, N-dimethyl-3-aminopropyl) trimethoxysilane of 2530-86-1, 2-isocyanate pyridine of 4737-19-3, 2-aminopyridine of 504-29-0 and cysteine of 52-90-4; the following parts are parts by mass.
Industrial pulp preparation: adding the waste paper board and water into a hydropulper, and crushing to obtain industrial paper pulp with fineness of 100 meshes and concentration of 5-8%;
preparation of polyamino tree-like product: 21 parts of ethylenediamine and 8.8 parts of pentaerythritol tetraacrylate are sequentially added into 6.5 parts of methanol, the mixture is reacted for 20 hours at 50 ℃, the methanol and the ethylenediamine are removed by reduced pressure distillation, the mixture is washed by ethyl acetate, and the mixture is dried in vacuum to obtain the polyamino tree-like product.
Example 1: preparation of an antistatic calcium sulfate floor substrate:
step 1: mixing and stirring 70 parts of calcium sulfate hemihydrate, 14 parts of tricalcium silicate, 12 parts of perlite and 4 parts of chopped carbon fiber for 30 minutes at 250rpm to obtain powder;
step 2: (1) Adding 10 parts of cyclodextrin into 100 parts of pure water, adding 8.8 parts of potassium hydroxide, and stirring for dissolution; at 50 ℃, adding 3 parts of 2-aminopyridine and 12 parts of cysteine; at 60 ℃, 14 parts of epichlorohydrin is added dropwise, the adding time is 0.5 hour, and the reaction is carried out for 1 hour; adjusting pH to be less than 5.3, adding absolute ethyl alcohol, standing, filtering, purifying and drying to obtain sulfhydryl cyclodextrin;
(2) 10 parts of polyamino tree-like product are added into 1000 parts of toluene, 1.5 parts of 2-chloroethyl isocyanate and 1.6 parts of 2-isocyanate pyridine are added at 0 ℃ and stirred for 10 hours; adding 3.4 parts of (N, N-dimethyl-3-aminopropyl) trimethoxysilane, 110 parts of N, N-dimethylacetamide and 100 parts of toluene, stirring for 2 days at 80 ℃, concentrating, adding acetone for precipitation, filtering, washing and drying to obtain an amine curing agent;
step 3: 1.6 parts of sulfhydryl cyclodextrin and 2.8 parts of amine curing agent are added into 76 parts of industrial paper pulp with 6 weight percent in sequence, and stirred for 15 minutes at 500 rpm; adding 100 parts of powder and 0.64 part of water reducer, and continuously stirring for 15 minutes; adding 12 parts of aqueous epoxy resin and 0.25 part of curing accelerator Uyhard-UR-300, and stirring for 10 minutes to obtain a substrate raw material; the water reducer consists of a polycarboxylate water reducer SP-409 and a naphthalene water reducer SSF-1000 in a mass ratio of 5:3;
step 4: pouring the substrate raw material into a mould, rolling for 30 minutes at room temperature and 1.5Mpa, and rolling for 20 minutes at 100 ℃ and 6 Mpa; rolling for 10 minutes at 140 ℃ and 12 Mpa; then steam curing for 5 hours, drying at 80 ℃ for 24 hours; to obtain the antistatic calcium sulfate floor base material.
Example 2: preparation of an antistatic calcium sulfate floor substrate:
step 1: mixing 65 parts of calcium sulfate hemihydrate, 15 parts of tricalcium silicate, 16 parts of perlite and 4 parts of chopped carbon fiber at 250rpm, and stirring for 30 minutes to obtain powder;
step 2: (1) Adding 10 parts of cyclodextrin into 100 parts of pure water, adding 8.8 parts of potassium hydroxide, and stirring for dissolution; at 50 ℃, adding 3 parts of 2-aminopyridine and 12 parts of cysteine; at 60 ℃, 14 parts of epichlorohydrin is added dropwise, the adding time is 0.5 hour, and the reaction is carried out for 1 hour; adjusting pH to be less than 5.3, adding absolute ethyl alcohol, standing, filtering, purifying and drying to obtain sulfhydryl cyclodextrin;
(2) 10 parts of polyamino tree-like product are added into 1000 parts of toluene, 1.5 parts of 2-chloroethyl isocyanate and 1.6 parts of 2-isocyanate pyridine are added at 0 ℃ and stirred for 10 hours; adding 3.4 parts of (N, N-dimethyl-3-aminopropyl) trimethoxysilane, 110 parts of N, N-dimethylacetamide and 100 parts of toluene, stirring for 2 days at 80 ℃, concentrating, adding acetone for precipitation, filtering, washing and drying to obtain an amine curing agent;
step 3: 1.8 parts of sulfhydryl cyclodextrin and 2.8 parts of amine curing agent are added into 76 parts of industrial paper pulp with 5 weight percent in sequence, and stirred for 15 minutes at 500 rpm; adding 100 parts of powder and 0.4 part of water reducer, and continuously stirring for 15 minutes; adding 12.5 parts of aqueous epoxy resin and 0.3 part of curing accelerator Uyhard-UR-300, and stirring for 10 minutes to obtain a substrate raw material; the water reducer consists of a polycarboxylate water reducer SP-409 and a naphthalene water reducer SSF-1000 in a mass ratio of 5:3;
step 4: pouring the substrate raw material into a mould, rolling for 30 minutes at room temperature and 1.5Mpa, and rolling for 20 minutes at 100 ℃ and 6 Mpa; rolling for 10 minutes at 140 ℃ and 12 Mpa; then steam curing for 5 hours, drying at 80 ℃ for 24 hours; to obtain the antistatic calcium sulfate floor base material.
Example 3: preparation of an antistatic calcium sulfate floor substrate:
step 1: 75 parts of calcium sulfate hemihydrate, 13 parts of tricalcium silicate, 10 parts of perlite and 2 parts of chopped carbon fiber are mixed and stirred for 30 minutes at 250rpm to obtain powder;
step 2: (1) Adding 10 parts of cyclodextrin into 100 parts of pure water, adding 8.8 parts of potassium hydroxide, and stirring for dissolution; at 50 ℃, adding 3 parts of 2-aminopyridine and 12 parts of cysteine; at 60 ℃, 14 parts of epichlorohydrin is added dropwise, the adding time is 0.5 hour, and the reaction is carried out for 1 hour; adjusting pH to be less than 5.3, adding absolute ethyl alcohol, standing, filtering, purifying and drying to obtain sulfhydryl cyclodextrin;
(2) 10 parts of polyamino tree-like product are added into 1000 parts of toluene, 1.5 parts of 2-chloroethyl isocyanate and 1.6 parts of 2-isocyanate pyridine are added at 0 ℃ and stirred for 10 hours; adding 3.4 parts of (N, N-dimethyl-3-aminopropyl) trimethoxysilane, 110 parts of N, N-dimethylacetamide and 100 parts of toluene, stirring for 2 days at 80 ℃, concentrating, adding acetone for precipitation, filtering, washing and drying to obtain an amine curing agent;
step 3: 1.2 parts of sulfhydryl cyclodextrin and 2.3 parts of amine curing agent are added into 80 parts of 8wt% industrial paper pulp in sequence, and stirred for 15 minutes at 500 rpm; adding 100 parts of powder and 0.8 part of water reducer, and continuously stirring for 15 minutes; adding 12.5 parts of aqueous epoxy resin and 0.2 part of curing accelerator Uyhard-UR-300, and stirring for 10 minutes to obtain a substrate raw material; the water reducer consists of a polycarboxylate water reducer SP-409 and a naphthalene water reducer SSF-1000 in a mass ratio of 5:3;
step 4: pouring the substrate raw material into a mould, rolling for 30 minutes at room temperature and 1.5Mpa, and rolling for 20 minutes at 100 ℃ and 6 Mpa; rolling for 10 minutes at 140 ℃ and 12 Mpa; then steam curing for 5 hours, drying at 80 ℃ for 24 hours; to obtain the antistatic calcium sulfate floor base material.
Comparative example 1: according to example 1, no tricalcium silicate was introduced into the meal, modified as: 84 parts of calcium sulfate hemihydrate, 12 parts of perlite and 4 parts of chopped carbon fiber are mixed and stirred for 30 minutes at 250rpm to obtain powder; the remainder being identical.
Comparative example 2: according to example 1, no mercaptocyclodextrin was introduced, modified as: 4.4 parts of an amine curing agent are added to 76 parts of 6wt% industrial pulp in sequence and stirred at 500rpm for 15 minutes; adding 100 parts of powder and 0.64 part of water reducer, and continuously stirring for 15 minutes; adding 12 parts of aqueous epoxy resin and 0.25 part of curing accelerator Uyhard-UR-300, and stirring for 10 minutes to obtain a substrate raw material; the remainder being identical.
Comparative example 3: according to example 1, the mercaptocyclodextrin was replaced with hepta (6-mercapto-6-deoxybetacyclodextrin (CAS number: 160661-60-9); the remainder being identical.
Comparative example 4: according to example 1, a single polycarboxylate water reducer SP-409 was used as the water reducer, the remainder being identical.
Comparative example 5: the polyamino tree product was used as amine curing agent according to example 1, the remainder being the same.
Performance test 1: the antistatic calcium sulfate floor base materials prepared in the examples and the comparative examples are subjected to strength and antistatic performance tests; 100X 20X 10mm 3 Using a bending and compression resistant integrated testing machine to detect the compression strength at 0.5 mm/min; referring to GB/T1410-2006, the surface resistivity is detected at 25℃at 65% RH; the data obtained are shown in the following table:
| sample of | Compressive strength (MPa) | Surface resistance (10) 5 Omega/square meter) |
| Example 1 | 30.7 | 7.38 |
| Example 2 | 29.5 | 7.51 |
| Example 3 | 29.1 | 7.57 |
| Comparative example 1 | 25.9 | 7.95 |
| Comparative example 2 | 26.6 | 8.87 |
| Comparative example 3 | 27.8 | 8.33 |
| Comparative example 4 | 28.6 | 7.65 |
| Comparative example 5 | 29.1 | 8.70 |
Conclusion: the experiment shows that the calcium sulfate floor substrate prepared in the scheme has excellent compressive strength, up to 30.7MPa, excellent antistatic performance and surface resistance as low as 7.38X10 5 Omega/square meter. Comparison of the data of example 1 with comparative examples 1-5 shows that: the compressive strength is effectively enhanced by introducing tricalcium silicate; the introduction of the sulfhydryl cyclodextrin effectively enhances the mechanical property and improves the antistatic property; compared with the seven (6-mercapto-6-deoxidized) beta cyclodextrin purchased from the market, the sulfhydryl cyclodextrin prepared in the application has better enhancement. In addition, the combined water reducer has increased compression strength due to increased compactness. In a further scheme, the polyamino tree-shaped product is further modified, so that the compression resistance and the antistatic performance are effectively enhanced.
Performance test 2: compounding the antistatic calcium sulfate floor substrate in the example 1 with the galvanized steel sheet ground surface and the melamine veneering, and conducting PVC edge sealing to prepare an antistatic movable floor; and performing performance detection on the alloy.
Results: the ground resistance of the anti-static movable floor is 5.26 multiplied by 10 8 Omega; the concentrated load deflection is: center point 0.98mm, edge center point 1.26, diagonal quarter point 0.71; the deflection of the uniformly distributed load is 0.67mm; the limit concentrated load is: center point 25630N, edge center point 14850N, diagonalThe four points of the line are: 18320N; the anti-static movable floor has excellent mechanical strength and anti-static performance.
Finally, it should be noted that: the foregoing description is only a preferred embodiment of the present application, and the present application is not limited thereto, but it is to be understood that modifications and equivalents of some of the technical features described in the foregoing embodiments may be made by those skilled in the art, although the present application has been described in detail with reference to the foregoing embodiments. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in the protection scope of the present application.
Claims (4)
1. The preparation method of the antistatic calcium sulfate floor substrate is characterized by comprising the following steps of: the method comprises the following steps:
step 1: mixing and stirring calcium sulfate hemihydrate, tricalcium silicate, perlite and chopped carbon fiber to obtain powder;
step 2: adding cyclodextrin into water, adding potassium hydroxide, and stirring for dissolving; adding 2-aminopyridine and cysteine at 50-55 ℃; at 60-65 ℃, epoxy chloropropane is added dropwise for reaction for 1-2 hours; adjusting the pH to be 5-6, adding absolute ethyl alcohol, standing, filtering, purifying and drying to obtain sulfhydryl cyclodextrin;
step 3: sequentially adding sulfhydryl cyclodextrin and amine curing agent into paper pulp, and uniformly mixing; adding powder and a water reducing agent, and stirring and mixing; adding the aqueous epoxy resin and the curing accelerator, and stirring and mixing to obtain a substrate raw material;
step 4: pouring the substrate raw material into a mould, and rolling and forming; steam curing and drying; obtaining the antistatic calcium sulfate floor base material;
the preparation method of the amine curing agent comprises the following steps: (1) Sequentially adding ethylenediamine and pentaerythritol tetraacrylate into methanol, reacting for 20-24 hours at 50-55 ℃, and performing reduced pressure distillation, washing and drying to obtain a polyamino tree-like product; (2) Adding the polyamino tree-like product into toluene, adding 2-chloroethyl isocyanate and isocyanate pyridine at 0-5 ℃, and stirring for 10-12 hours; adding (N, N-dimethyl-3-aminopropyl) trimethoxysilane, N-dimethylacetamide and toluene, stirring for 2-3 days at 80-85 ℃, purifying and drying to obtain an amine curing agent;
the substrate raw materials comprise the following components: 100 parts of powder, 76-80 parts of paper pulp, 0.4-0.8 part of water reducer, 7.5-12.5 parts of water-based epoxy resin, 2.3-2.8 parts of amine curing agent, 1.2-1.8 parts of sulfhydryl cyclodextrin and 0.2-0.3 part of curing accelerator;
the raw materials of the sulfhydryl cyclodextrin comprise the following components: 10 parts of cyclodextrin, 2.5-3.5 parts of 2-aminopyridine, 11-13 parts of cysteine and 13-15 parts of epichlorohydrin;
the powder comprises the following components: 65-75 parts of calcium sulfate hemihydrate, 13-15 parts of tricalcium silicate, 10-16 parts of perlite and 2-4 parts of chopped carbon fiber in parts by weight;
the water reducer consists of a polycarboxylate water reducer and a naphthyl water reducer in a mass ratio of 5:3;
the amine curing agent comprises, by weight, 10 parts of polyamino tree-like products, 1.4-1.6 parts of 2-chloroethyl isocyanate, 1.5-1.8 parts of isocyanate pyridine and 3.2-3.5 parts of (N, N-dimethyl-3-aminopropyl) trimethoxysilane.
2. The method for preparing the antistatic calcium sulfate floor substrate according to claim 1, wherein the method comprises the following steps: the pulp is industrial pulp with the weight of 5-8wt%.
3. The method for preparing the antistatic calcium sulfate floor substrate according to claim 1, wherein the method comprises the following steps: the rolling forming process comprises the following steps: rolling for 20-30 minutes at room temperature under 1-2 mpa, and rolling for 20-30 minutes at 80-100 ℃ under 5-8 mpa; rolling for 10-15 minutes at 120-140 ℃ and 10-12 mpa; the steam curing time is 3-5 hours; the drying conditions are as follows: and drying at 60-100 ℃ for 20-30 hours.
4. The antistatic calcium sulfate floor substrate prepared by the preparation method of the antistatic calcium sulfate floor substrate according to any one of claims 1-3.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108191366A (en) * | 2017-12-25 | 2018-06-22 | 安徽向利机房设备工程有限公司 | A kind of calcium sulfate antistatic floor and preparation method thereof |
| CN112250410A (en) * | 2020-10-22 | 2021-01-22 | 湖北吉佩克环保科技有限公司 | Antistatic plate using industrial byproduct gypsum as raw material and preparation method thereof |
| CN113912336A (en) * | 2021-11-02 | 2022-01-11 | 江苏横山南方水泥有限公司 | Special cement filling material for anti-static floor, preparation method and application |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108191366A (en) * | 2017-12-25 | 2018-06-22 | 安徽向利机房设备工程有限公司 | A kind of calcium sulfate antistatic floor and preparation method thereof |
| CN112250410A (en) * | 2020-10-22 | 2021-01-22 | 湖北吉佩克环保科技有限公司 | Antistatic plate using industrial byproduct gypsum as raw material and preparation method thereof |
| CN113912336A (en) * | 2021-11-02 | 2022-01-11 | 江苏横山南方水泥有限公司 | Special cement filling material for anti-static floor, preparation method and application |
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Denomination of invention: An anti-static calcium sulfate floor substrate and its preparation method Granted publication date: 20231024 Pledgee: Bank of China Limited Changzhou Economic Development Zone sub branch Pledgor: Changzhou Abete machine room equipment Co.,Ltd. Registration number: Y2024980008832 |