CN115838443A - Sulfonated guar gum ether and preparation method and application thereof - Google Patents
Sulfonated guar gum ether and preparation method and application thereof Download PDFInfo
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- CN115838443A CN115838443A CN202211468964.XA CN202211468964A CN115838443A CN 115838443 A CN115838443 A CN 115838443A CN 202211468964 A CN202211468964 A CN 202211468964A CN 115838443 A CN115838443 A CN 115838443A
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- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 title claims abstract description 100
- 229920002907 Guar gum Polymers 0.000 title claims abstract description 42
- 239000000665 guar gum Substances 0.000 title claims abstract description 42
- 235000010417 guar gum Nutrition 0.000 title claims abstract description 42
- 229960002154 guar gum Drugs 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 39
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000006277 sulfonation reaction Methods 0.000 claims abstract description 17
- 239000003054 catalyst Substances 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 7
- DZSVIVLGBJKQAP-UHFFFAOYSA-N 1-(2-methyl-5-propan-2-ylcyclohex-2-en-1-yl)propan-1-one Chemical group CCC(=O)C1CC(C(C)C)CC=C1C DZSVIVLGBJKQAP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000004570 mortar (masonry) Substances 0.000 claims description 44
- 244000007835 Cyamopsis tetragonoloba Species 0.000 claims description 27
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 11
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical group CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 claims description 7
- 230000008569 process Effects 0.000 claims description 7
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 150000002170 ethers Chemical class 0.000 claims description 5
- 238000006386 neutralization reaction Methods 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000006467 substitution reaction Methods 0.000 abstract description 15
- 206010016807 Fluid retention Diseases 0.000 description 18
- 230000000052 comparative effect Effects 0.000 description 18
- 239000000203 mixture Substances 0.000 description 16
- -1 carboxymethyl hydroxypropyl Chemical class 0.000 description 11
- 229910052739 hydrogen Inorganic materials 0.000 description 11
- 239000001257 hydrogen Substances 0.000 description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 8
- 229920003086 cellulose ether Polymers 0.000 description 8
- 229920013818 hydroxypropyl guar gum Polymers 0.000 description 7
- 230000008719 thickening Effects 0.000 description 7
- 239000000843 powder Substances 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 238000001228 spectrum Methods 0.000 description 6
- 239000003638 chemical reducing agent Substances 0.000 description 5
- 239000010881 fly ash Substances 0.000 description 5
- 229920003023 plastic Polymers 0.000 description 5
- 239000004033 plastic Substances 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 239000004568 cement Substances 0.000 description 4
- 230000007613 environmental effect Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- 239000004576 sand Substances 0.000 description 4
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 description 4
- 125000000542 sulfonic acid group Chemical group 0.000 description 4
- 229920000536 2-Acrylamido-2-methylpropane sulfonic acid Polymers 0.000 description 3
- XHZPRMZZQOIPDS-UHFFFAOYSA-N 2-Methyl-2-[(1-oxo-2-propenyl)amino]-1-propanesulfonic acid Chemical compound OS(=O)(=O)CC(C)(C)NC(=O)C=C XHZPRMZZQOIPDS-UHFFFAOYSA-N 0.000 description 3
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 description 3
- 239000004354 Hydroxyethyl cellulose Substances 0.000 description 3
- 235000001484 Trigonella foenum graecum Nutrition 0.000 description 3
- 244000250129 Trigonella foenum graecum Species 0.000 description 3
- 229920002522 Wood fibre Polymers 0.000 description 3
- 229960000583 acetic acid Drugs 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 238000010276 construction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- 239000012362 glacial acetic acid Substances 0.000 description 3
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 description 3
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 description 3
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 description 3
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 description 3
- UFVKGYZPFZQRLF-UHFFFAOYSA-N hydroxypropyl methyl cellulose Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(O)C(CO)O3)O)C(CO)O2)O)C(CO)O1 UFVKGYZPFZQRLF-UHFFFAOYSA-N 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 235000001019 trigonella foenum-graecum Nutrition 0.000 description 3
- 239000002025 wood fiber Substances 0.000 description 3
- OMDQUFIYNPYJFM-XKDAHURESA-N (2r,3r,4s,5r,6s)-2-(hydroxymethyl)-6-[[(2r,3s,4r,5s,6r)-4,5,6-trihydroxy-3-[(2s,3s,4s,5s,6r)-3,4,5-trihydroxy-6-(hydroxymethyl)oxan-2-yl]oxyoxan-2-yl]methoxy]oxane-3,4,5-triol Chemical compound O[C@@H]1[C@@H](O)[C@@H](O)[C@@H](CO)O[C@@H]1OC[C@@H]1[C@@H](O[C@H]2[C@H]([C@@H](O)[C@H](O)[C@@H](CO)O2)O)[C@H](O)[C@H](O)[C@H](O)O1 OMDQUFIYNPYJFM-XKDAHURESA-N 0.000 description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 2
- 244000303965 Cyamopsis psoralioides Species 0.000 description 2
- 229920000926 Galactomannan Polymers 0.000 description 2
- 229920001479 Hydroxyethyl methyl cellulose Polymers 0.000 description 2
- 244000275012 Sesbania cannabina Species 0.000 description 2
- 229920001938 Vegetable gum Polymers 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 125000003368 amide group Chemical group 0.000 description 2
- 239000004567 concrete Substances 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 238000009415 formwork Methods 0.000 description 2
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 2
- 230000010354 integration Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229920000609 methyl cellulose Polymers 0.000 description 2
- 239000001923 methylcellulose Substances 0.000 description 2
- 235000010981 methylcellulose Nutrition 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 230000003472 neutralizing effect Effects 0.000 description 2
- 239000002893 slag Substances 0.000 description 2
- 235000010288 sodium nitrite Nutrition 0.000 description 2
- BWYYYTVSBPRQCN-UHFFFAOYSA-M sodium;ethenesulfonate Chemical group [Na+].[O-]S(=O)(=O)C=C BWYYYTVSBPRQCN-UHFFFAOYSA-M 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 2
- AKEJUJNQAAGONA-UHFFFAOYSA-N sulfur trioxide Chemical compound O=S(=O)=O AKEJUJNQAAGONA-UHFFFAOYSA-N 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000002562 thickening agent Substances 0.000 description 2
- CLHYKAZPWIRRRD-UHFFFAOYSA-N 1-hydroxypropane-1-sulfonic acid Chemical compound CCC(O)S(O)(=O)=O CLHYKAZPWIRRRD-UHFFFAOYSA-N 0.000 description 1
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- GAWIXWVDTYZWAW-UHFFFAOYSA-N C[CH]O Chemical group C[CH]O GAWIXWVDTYZWAW-UHFFFAOYSA-N 0.000 description 1
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 239000011398 Portland cement Substances 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000002057 carboxymethyl group Chemical group [H]OC(=O)C([H])([H])[*] 0.000 description 1
- 239000011083 cement mortar Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000006266 etherification reaction Methods 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000010440 gypsum Substances 0.000 description 1
- 229910052602 gypsum Inorganic materials 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 239000012744 reinforcing agent Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910021487 silica fume Inorganic materials 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000007655 standard test method Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- HIFJUMGIHIZEPX-UHFFFAOYSA-N sulfuric acid;sulfur trioxide Chemical group O=S(=O)=O.OS(O)(=O)=O HIFJUMGIHIZEPX-UHFFFAOYSA-N 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
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- 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
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- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention provides sulfonated guar gum ether and a preparation method and application thereof. The sulfonated guar gum ether comprises the following raw materials in parts by weight: 100 parts of guar gum, 60-150 parts of water, 5-30 parts of a sulfonation reagent, 5-30 parts of an etherifying agent and 3-15 parts of a catalyst; the sulfonation reagent is 2-acrylamide-2-methylpropanesulfonic acid. The sulfonated guar gum ether has low substitution degree, high viscosity and good water retention.
Description
Technical Field
The invention belongs to the technical field of dry-mixed mortar, and relates to sulfonated guar gum ether, and a preparation method and application thereof.
Background
The dry-mixed mortar belongs to commercial mortar, is named as premixed (dry) mortar at first in China according to the name of national standard GB/T25181-2019 'premixed mortar', is named as dry powder, dry mixture, dry powder mortar or dry-mixed mortar at later time, is composed of solid materials such as cementing materials, mineral admixtures, fine aggregates, additives and the like, and is a semi-finished mortar prepared by factory batching and mixing and does not contain mixing water. Dry-mixed mortars appeared in austria at the end of the 19 th century, and europe experienced over 50 years of history from inventing to large-scale production and use of dry-mixed mortars. With the continuous improvement of the requirements of the global building industry on the building process, the building engineering puts higher requirements on the strength, functionality, durability and the like of the building mortar, and the development and application of the dry-mixed mortar are gradually developed in the world. Through the development of short time in China, the superiority of the dry-mixed mortar in the aspects of quality, efficiency, economy, environmental protection and the like is increasingly shown, and the corresponding research is gradually expanded.
The dry-mixed mortar consists of 3 main components, such as a cementing material, aggregate, an additive and the like. According to different purposes, dry-mixed mortar with different functions can be prepared according to different formulas. Wherein, the cementing material of the dry-mixed mortar mainly plays a role in cementing, and comprises cement, lime, gypsum and the like; the aggregate mainly plays a role of a skeleton, and comprises sand, inert powder and the like; the additive mainly improves the workability and stability of the mortar, has small addition amount but has huge effect, and comprises high molecular polymers (redispersible polymers, cellulose ether, guar gum ether, polyvinyl alcohol and the like), pigments, fibers and the like.
The high molecular polymer cellulose ether in the dry-mixed mortar has good water retention and thickening effects, can obviously improve the workability of cement mortar, and is the most commonly used high molecular polymer, and comprises Methylcellulose (MC), hydroxyethyl cellulose (HEC), hydroxyethyl methylcellulose (HEMC), hydroxypropyl methylcellulose (HPMC) and the like.
Guar ethers function in dry-mixed mortars for thickening and water retention, similar to cellulose ethers. It is a high cost performance water retention and thickening material, and is used to replace expensive cellulose ether.
CN102363637A discloses a preparation method and application of a thickening water-retaining agent for building dry-mixed mortar, wherein the preparation method comprises the following steps: (1) Mixing guar gum raw powder, a solvent and a surfactant to obtain a mixed solution; (2) Adding a catalyst into the mixed solution obtained in the step (1), introducing nitrogen, and carrying out an alkalization reaction at room temperature; (3) Adding etherifying agent for etherification, wherein the pressure is 0.3-0.4MPa, the temperature is 40-90 ℃, preferably 50-70 ℃, and the time is 2-5 hours, preferably 3-4 hours; (4) Cooling to 25-40 ℃, adding a neutralizing agent until the pH value of the system is 6-8, and then collecting the thickening water-retaining agent from the reaction product. The thickening water-retaining agent for the building dry-mixed mortar can endow good water retention property and workability when being applied to the building dry-mixed mortar; meanwhile, the price of the thickening water-retaining agent is obviously lower than that of the cellulose ether, and the complete or partial substitution of the cellulose ether can obviously reduce the formula cost of the product.
CN106977130A discloses a mortar water-retaining thickener, which comprises diatomite, fly ash, an air-entraining agent, guar gum ether, a water reducing agent and sulfonate; the diatomite water reducing agent comprises, by weight, 1.0-1.5 parts of fly ash, 0.5-1.0 part of air entraining agent, 0.2-0.8 part of guar gum ether, 0.2-0.5 part of water reducing agent and 0.2-0.5 part of sulfonate, wherein relative to 1 part of diatomite, the content of the fly ash is 1.0-1.5 parts, the content of the air entraining agent is 0.5-1.0 part, and the content of the guar gum ether is 0.2-0.8 part. The mortar water-retention thickening agent disclosed by the invention not only meets the requirements of water absorption rate, flame retardant rate, strength and the like, but also has the advantages of improving construction quality, avoiding wall body cracking, simple preparation method, high operability, greenness, environmental friendliness and higher economic and social values.
CN104496296A discloses a dry-mixed waterproof and antifreezing mortar and a preparation method thereof, wherein the dry-mixed waterproof and antifreezing mortar contains cement, fly ash, phosphorous slag, river sand, wood fiber, guar gum ether, a water reducing agent, an early strength agent and sodium nitrite; relative to 100 parts by weight of river sand, the cement content is 15-25 parts by weight, the fly ash content is 10-15 parts by weight, the phosphorous slag content is 5-8 parts by weight, the wood fiber content is 3-6 parts by weight, the guar gum ether content is 4-7 parts by weight, the water reducing agent content is 0.3-0.5 part by weight, the early strength agent content is 0.5-0.8 part by weight, and the sodium nitrite content is 1-3 parts by weight. The dry-mixed waterproof and antifreezing mortar can be used in cold environment and has no cracking and peeling.
CN111908863A discloses a plastic formwork concrete wall plastering mortar and a preparation method thereof, and the preparation method comprises the steps of adding silica fume, anti-crack fibers, titanate, hydroxypropyl methyl cellulose, hydroxypropyl guar gum ether, rubber powder and cement into water, and stirring to obtain the plastic formwork concrete wall plastering mortar; the raw materials are added stage by stage, so that the dispersibility of the inorganic components is improved, the components are uniformly dispersed to influence the plastering performance of the mortar when being used as a mixture, the uniform and fine mortar is easy to paint, and the adhesion is good after drying. By researching the plastering technology, the invention solves the problems of smooth molding surface of the plastic mould, difficult plastering adhesion, shortened construction period, reduced cost, driving the use of the plastic mould in the construction industry and solving the problem of low mortar adhesion strength of the existing plastic mould.
CN103113486B discloses sulfonic acid modified carboxymethyl hydroxypropyl guar gum and a preparation method and application thereof, wherein the sulfonic acid modified carboxymethyl hydroxypropyl guar gum has the following structural formula:
wherein R = H, n =0,1,2 or 3; or R = OH, n =0-6. The application specifically refers to the application of the fracturing fluid in preparation of fracturing fluid.
CN106146677A discloses a preparation method of dry sulfonic hydroxypropyl guar gum, which adopts 3-chloro-2-sodium hydroxypropanesulfonate as a sulfonation reagent, and the sulfonic hydroxypropyl guar gum can be used as a reinforcing agent, a retention aid, a filter aid and an adhesive.
CN107522791B discloses a vegetable gum containing sulfonic acid groups, wherein the sulfonic acid groups are located at any hydroxyl sites of galactomannan and derivatives thereof, the galactomannan and derivatives thereof are selected from at least one of guar gum, fenugreek gum, sesbania gum, hydroxypropyl guar gum, carboxymethyl hydroxypropyl guar gum, hydroxypropyl fenugreek gum, carboxymethyl fenugreek gum and hydroxyethyl sesbania gum, and the degree of substitution of the sulfonic acid groups is 0.20-0.80. The sulfonating agent is selected from fuming sulfuric acid and/or sulfur trioxide. The vegetable gum containing sulfonic acid groups is used for preparing fracturing fluid.
However, the reaction degree of the sulfonation reagent adopted in the above preparation method is severe and is not easy to control, and the water retention performance of the prepared sulfonated guar gum ether needs to be further improved.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide sulfonated guar gum ether and a preparation method and application thereof.
One of the purposes of the invention is to provide a sulfonated guar gum ether, and the invention adopts the following technical scheme for achieving the purpose:
the sulfonated guar gum ether comprises the following raw materials in parts by weight:
the sulfonation reagent is 2-acrylamide-2-methylpropanesulfonic acid.
According to the sulfonated guar gum ether, water is used as a solvent, so that the production cost and the environmental protection pressure are greatly reduced; the etherifying agent and the sulfonating reagent are used in small amount, the cost is low, the reaction requirement is reduced, the hydroxypropyl substitution degree range of the sulfonated guar gum ether prepared by adopting 2-acrylamide-2-methylpropanesulfonic acid as the sulfonating reagent is 0.1-0.3, the sulfonic substitution degree range is 0.1-0.3, the sulfonated guar gum ether belongs to a product with lower substitution degree, the viscosity is high, and the water retention is good.
Specifically, the sulfonated guar gum ether comprises the following raw materials in parts by weight:
the weight portion of the guar gum is 100 portions.
The water is 60 to 150 parts by weight, for example, 60 parts, 65 parts, 70 parts, 75 parts, 80 parts, 85 parts, 90 parts, 95 parts, 100 parts, 105 parts, 110 parts, 115 parts, 120 parts, 125 parts, 130 parts, 135 parts, 140 parts, 145 parts, 150 parts, or the like.
The sulfonation reagent is present in an amount of 5 to 30 parts by weight, for example, 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, 10 parts, 11 parts, 12 parts, 13 parts, 14 parts, 15 parts, 16 parts, 17 parts, 18 parts, 19 parts, 20 parts, 21 parts, 22 parts, 23 parts, 24 parts, 25 parts, 26 parts, 27 parts, 28 parts, 29 parts, 30 parts, and the like.
The etherifying agent is 5 to 30 parts by weight, for example, 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, 10 parts, 11 parts, 12 parts, 13 parts, 14 parts, 15 parts, 16 parts, 17 parts, 18 parts, 19 parts, 20 parts, 21 parts, 22 parts, 23 parts, 24 parts, 25 parts, 26 parts, 27 parts, 28 parts, 29 parts, 30 parts, etc.
The catalyst is present in an amount of 3 to 15 parts by weight, for example 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14 or 15 parts by weight.
In the invention, the sulfonation reagent is 2-acrylamide-2-methylpropanesulfonic acid. 2-acrylamide-2-methylpropanesulfonic acid is used as a sulfonation reagent, and compared with other types of sulfonation reagents, the sulfonation reagent adopted in the invention has mild reaction and easily controlled reaction process.
In the invention, the etherifying agent is propylene oxide or ethylene oxide. Compared with other types of etherifying agents, the etherifying agent adopts propylene oxide or ethylene oxide as the etherifying agent, the reaction is milder, and the reaction process is easy to control.
In the invention, the catalyst is sodium hydroxide or potassium hydroxide.
The reaction formula of the sulfonated guar ethers of the present invention is as follows:
the second object of the present invention is to provide a process for the preparation of sulfonated guar ethers according to the first object, comprising the following steps:
mixing guar gum with water according to a ratio, adding a sulfonation reagent, an etherifying agent and a catalyst for reaction, cooling after the reaction is finished, adding acid for neutralization, and drying in vacuum to obtain the sulfonated guar gum ether.
Wherein the reaction time is 1-3 hours, such as 1 hour, 1.5 hours, 2 hours, 2.5 hours, 3 hours; the reaction temperature is 50-80 deg.C, such as 50 deg.C, 55 deg.C, 60 deg.C, 65 deg.C, 70 deg.C, 75 deg.C or 80 deg.C.
Wherein the temperature of the cooling is 35-45 deg.C, such as 35 deg.C, 36 deg.C, 37 deg.C, 38 deg.C, 39 deg.C, 40 deg.C, 41 deg.C, 42 deg.C, 43 deg.C, 44 deg.C or 45 deg.C.
Wherein, the acid is adopted for neutralization.
The invention also aims to provide the application of the sulfonated guar ether, which is one of the aims, and the sulfonated guar ether is used for preparing dry-mixed mortar.
The invention also aims to provide a dry-mixed mortar, which comprises the sulfonated guar ether of one of the purposes, and the dry-mixed mortar comprises the following components in percentage by weight:
specifically, the dry-mixed mortar comprises the following components in percentage by weight:
the silica sand is 50 to 70% by weight, for example, 50%, 51%, 52%, 53%, 54%, 55%, 56%, 57%, 58%, 59%, 60%, 61%, 62%, 63%, 64%, 65%, 66%, 67%, 68%, 69%, 70%, or the like.
The Portland cement is 30 to 40% by weight, for example, 30%, 31%, 32%, 33%, 34%, 35%, 36%, 37%, 38%, 39%, 40%, or the like.
The wood fibers are present in an amount of 0.1 to 1% by weight, for example 0.1%, 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, or 1%.
The weight percentage of sulfonated guar ether is 0.1-1%, for example 0.1%, 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, or 1%, etc.
The percentage by weight of the dispersion rubber powder is 2 to 5%, for example 2%, 2.5%, 3%, 3.5%, 4%, 4.5%, 5%.
Compared with the prior art, the invention has the beneficial effects that:
according to the sulfonated guar gum ether, water is used as a solvent, so that the production cost and the environmental protection pressure are greatly reduced; the etherifying agent and the sulfonating agent are used in small amount, the cost is low, the reaction requirement is reduced, the hydroxypropyl substitution degree range of the prepared sulfonated guar gum ether is 0.1-0.3, the sulfonic substitution degree range is 0.1-0.3, the sulfonated guar gum ether belongs to a product with lower substitution degree, the viscosity is high, the viscosity of 2% solution is 25700-26100cp, the water retention is good, and the water retention rate of the prepared dry-mixed mortar is 96.1-99.3%.
Drawings
Fig. 1 is a nuclear magnetic hydrogen spectrum of the raw guar gum of the present invention;
FIG. 2 is a nuclear magnetic hydrogen spectrum of a sulfonated guar ether made according to the present invention;
fig. 3 is a nuclear magnetic hydrogen spectrum of the raw guar gum ether of the present invention.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments.
Unless otherwise specified, various starting materials of the present invention are commercially available or prepared according to conventional methods in the art.
Example 1
The sulfonated guar ether of this example was prepared as follows:
100 g of guar gum (shown in a nuclear magnetic hydrogen spectrum figure 1) and 90g of water are added into a small kneader and mixed, the mixture is vacuumized to remove air, nitrogen is filled, 12 g of sodium hydroxide and 20 g of 2-acrylamido-2-methylpropanesulfonic acid are added, the mixture is stirred for 15 minutes, then the mixture is heated to 70 ℃ and is kept warm for 1 hour, 18 g of propylene oxide is added dropwise, the temperature is kept for 1 hour at 70 ℃, the mixture is cooled to room temperature and neutralized to alkalescence by adding glacial acetic acid. And (3) drying the neutralized mixture in vacuum, and crushing to obtain sulfonated guar gum ether A, wherein the nuclear magnetic hydrogen spectrum of the sulfonated guar gum ether A is shown in figure 2.
As can be seen from FIG. 2, the peak at 2.5ppm is the peak at hydrogen on methylene linked to the amide group on the sulfonating agent, the peak at 1.2ppm is the peak at hydrogen on methyl linked to the amide group on the sulfonating agent, and the peak at 0.9ppm is the peak at methyl hydrogen of the etherifying agent, and the sulfonation substitution degree is 0.17 and the hydroxypropyl substitution degree is 0.27 as calculated by the integration of the peaks.
Viscosity measurements the viscosity of the 2% solution of sulfonated guar ether-like A prepared in this example at 25 ℃ was 26100cp using a Brookfield viscometer (20 rpm).
Example 2
The sulfonated guar ether of this example was prepared as follows:
adding 100 g of guar gum and 80g of water into a small kneader, mixing, vacuumizing to remove air, introducing nitrogen, adding 10g of sodium hydroxide and 15 g of 2-acrylamido-2-methylpropanesulfonic acid, stirring for 15 minutes, heating to 65 ℃, keeping the temperature for 1 hour, dropwise adding 15 g of propylene oxide, keeping the temperature for 1 hour at 65 ℃, cooling the mixture to room temperature, and neutralizing to alkalescence by adding glacial acetic acid. And (4) drying the neutralized mixture in vacuum, and crushing to obtain the sulfonated guar ether-like B.
The sulfonated guar ether-like B prepared in this example had a sulfonated degree of substitution of 0.12, a hydroxypropyl degree of substitution of 0.20, and a viscosity of 23200cp (Brookfield viscometer, 20 rpm) in a 2% solution at 25 ℃.
Comparative example 1
The guar ether of this comparative example was prepared as follows:
100 g of guar gum and 110g of water are added into a small kneader and mixed, the mixture is vacuumized to remove air, nitrogen is filled, 5 g of sodium hydroxide is added, the mixture is stirred for 15 minutes, then the mixture is heated to 70 ℃ and is kept warm for 1 hour, 18 g of propylene oxide is added dropwise, the mixture is kept warm for 1 hour at 70 ℃, the mixture is cooled to room temperature and neutralized to alkalescence by adding glacial acetic acid. And (3) drying the neutralized mixture in vacuum, and crushing to obtain guar ether-like C, wherein the nuclear magnetic hydrogen spectrum of the guar ether-like C is shown in figure 3.
As can be seen from fig. 3, the peak at 0.9ppm is the spectral peak of methyl hydrogen of the etherifying agent, and the hydroxypropyl degree of substitution of guar ether-like C calculated by integration of the peaks is 0.30.
Guar ether-like C has a viscosity of 26500cp (Brookfield viscometer, 20 rpm) in a 2% solution at 25 ℃.
Application example
The prepared sulfonated guar gum ether A, sulfonated guar gum ether B, guar gum ether C and a commercial cellulose ether product HEC28000 are used as raw materials to respectively prepare dry-mixed mortar, and the specific formula is shown in Table 1.
TABLE 1
The prepared dry-mixed mortar is mixed with 20% of water and then is filled into a test mould, and the respective water retention rates W are tested and compared according to the method of JGJ/T70-2009 Standard test method for basic performance of building mortar. The test data are shown in table 2.
TABLE 2
As can be seen from the data in table 2, the water retention of the sulfonated guar ether is better than that of the guar ether at the same addition amount, and the sulfonated guar ether has the same excellent water retention effect as the commercially available cellulose ether HEC 28000.
Example 3
This example is different from example 1 in that the etherifying agent is replaced with ethylene oxide, and the rest is the same as example 1.
Comparative example 2
This comparative example differs from example 1 in that the sulfonating agent was used in an amount of 2 grams, all other things being equal to example 1.
Comparative example 3
This comparative example differs from example 1 in that the sulfonating agent was used in an amount of 50 g, and the others were the same as in example 1.
Comparative example 4
This comparative example differs from example 1 in that the amount of etherifying agent used is 1 gram, and is otherwise the same as example 1.
Comparative example 5
This comparative example is different from example 1 in that the etherifying agent is used in an amount of 30 g, and the rest is the same as in example 1.
Comparative example 6
This comparative example differs from example 1 in that the sulfonation reagent was replaced with sodium vinyl sulfonate, all other things being equal to example 1.
The sulfonated guar ethers obtained in example 3 and comparative examples 2 to 6 were used to prepare dry-mixed mortars according to the formulation shown in Table 1, and the performance tests were carried out, the results of which are shown in Table 3.
TABLE 3
As can be seen from table 3, example 1, which uses 2-acrylamido-2-methylpropanesulfonic acid as the sulfonation reagent, has a higher viscosity and better water retention than the sulfonated guar ether prepared by comparative example 6, which uses sodium vinylsulfonate as the sulfonation reagent.
The example 1 has better water retention rate by using propylene oxide as an etherifying agent compared with the sulfonated guar gum ether prepared by using ethylene oxide as an etherifying agent in the example 3.
Comparative example 2 too little sulfonating agent was used, resulting in a decrease in water retention.
Comparative example 3 too much sulfonating agent was used to lower the viscosity and water retention.
Comparative example 4 too little etherifying agent is used, resulting in a decrease in water retention.
Comparative example 5 too much etherifying agent is used, resulting in a decrease in viscosity and a decrease in water retention.
The present invention is illustrated by the above-mentioned examples, but the present invention is not limited to the above-mentioned detailed process equipment and process flow, i.e. it is not meant to imply that the present invention must rely on the above-mentioned detailed process equipment and process flow to be practiced. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are all within the protection scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.
Claims (10)
1. The sulfonated guar ether is characterized by comprising the following raw materials in parts by weight:
the sulfonation reagent is 2-acrylamide-2-methylpropanesulfonic acid.
2. The sulfonated guar ether according to claim 1, characterized in that the etherifying agent is propylene oxide or ethylene oxide.
3. The sulfonated guar ether according to claim 1, characterized in that the catalyst is sodium hydroxide or potassium hydroxide.
4. Process for the preparation of sulfonated guar ethers according to any one of claims 1 to 3, characterized in that it comprises the following steps:
mixing guar gum with water according to a ratio, adding a sulfonation reagent, an etherifying agent and a catalyst for reaction, cooling after the reaction is finished, adding acid for neutralization, and drying in vacuum to obtain the sulfonated guar gum ether.
5. The method according to claim 4, wherein the reaction time is 1 to 3 hours, and the reaction temperature is 50 to 80 ℃.
6. The method of claim 4, wherein the reduced temperature is 35-45 ℃.
7. The method according to claim 4, wherein the acid-addition neutralization is carried out using acetic acid.
8. Use of a sulfonated guar ether according to any one of claims 1 to 3, for the preparation of dry-mixed mortars.
9. A dry-mixed mortar, characterized in that it comprises a sulfonated guar ether according to any one of claims 1 to 3.
10. The dry-mixed mortar of claim 9, characterized by comprising, in weight percent:
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| CN103113486A (en) * | 2013-02-18 | 2013-05-22 | 中国石油天然气股份有限公司 | Sulfonic acid modified carboxymethyl hydroxypropyl guar gum and preparation method and application thereof |
| CN104277138A (en) * | 2014-10-30 | 2015-01-14 | 山东广浦生物科技有限公司 | Method for preparing carboxymethyl hydroxyalkyl guar gum powder by virtue of one-step etherification |
| CN108047348A (en) * | 2017-12-18 | 2018-05-18 | 苏州昕能胶体技术有限公司 | A kind of high substitution hydroxypropyl guar gum and its preparation method and application |
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| CN103113486A (en) * | 2013-02-18 | 2013-05-22 | 中国石油天然气股份有限公司 | Sulfonic acid modified carboxymethyl hydroxypropyl guar gum and preparation method and application thereof |
| CN104277138A (en) * | 2014-10-30 | 2015-01-14 | 山东广浦生物科技有限公司 | Method for preparing carboxymethyl hydroxyalkyl guar gum powder by virtue of one-step etherification |
| CN108047348A (en) * | 2017-12-18 | 2018-05-18 | 苏州昕能胶体技术有限公司 | A kind of high substitution hydroxypropyl guar gum and its preparation method and application |
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