CN115838443B - 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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- CN115838443B CN115838443B CN202211468964.XA CN202211468964A CN115838443B CN 115838443 B CN115838443 B CN 115838443B CN 202211468964 A CN202211468964 A CN 202211468964A CN 115838443 B CN115838443 B CN 115838443B
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- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 title claims abstract description 102
- 229920002907 Guar gum Polymers 0.000 title claims abstract description 45
- 239000000665 guar gum Substances 0.000 title claims abstract description 45
- 235000010417 guar gum Nutrition 0.000 title claims abstract description 45
- 229960002154 guar gum Drugs 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 47
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 10
- 229920000536 2-Acrylamido-2-methylpropane sulfonic acid Polymers 0.000 claims abstract description 8
- XHZPRMZZQOIPDS-UHFFFAOYSA-N 2-Methyl-2-[(1-oxo-2-propenyl)amino]-1-propanesulfonic acid Chemical group OS(=O)(=O)CC(C)(C)NC(=O)C=C XHZPRMZZQOIPDS-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000003054 catalyst Substances 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 239000004570 mortar (masonry) Substances 0.000 claims description 46
- 244000007835 Cyamopsis tetragonoloba Species 0.000 claims description 21
- 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
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 9
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical group CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 7
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 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
- 238000001291 vacuum drying Methods 0.000 claims description 5
- 229920002522 Wood fibre Polymers 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 238000006386 neutralization reaction Methods 0.000 claims description 4
- 239000002025 wood fiber Substances 0.000 claims description 4
- 239000006004 Quartz sand Substances 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000003469 silicate cement Substances 0.000 claims 1
- 238000006467 substitution reaction Methods 0.000 abstract description 14
- 238000006277 sulfonation reaction Methods 0.000 abstract description 11
- 230000000052 comparative effect Effects 0.000 description 18
- 239000000203 mixture Substances 0.000 description 18
- 206010016807 Fluid retention Diseases 0.000 description 16
- -1 carboxymethyl hydroxypropyl Chemical class 0.000 description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 229920003086 cellulose ether Polymers 0.000 description 8
- 239000001257 hydrogen Substances 0.000 description 7
- 229910052739 hydrogen Inorganic materials 0.000 description 7
- 229920013818 hydroxypropyl guar gum Polymers 0.000 description 7
- 238000000034 method Methods 0.000 description 7
- 238000001228 spectrum Methods 0.000 description 7
- 239000003638 chemical reducing agent Substances 0.000 description 6
- 230000008719 thickening Effects 0.000 description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- 239000010881 fly ash Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- IANQTJSKSUMEQM-UHFFFAOYSA-N 1-benzofuran Chemical compound C1=CC=C2OC=CC2=C1 IANQTJSKSUMEQM-UHFFFAOYSA-N 0.000 description 4
- 229960000583 acetic acid Drugs 0.000 description 4
- 239000004568 cement Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 230000007613 environmental effect Effects 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 229920003023 plastic Polymers 0.000 description 4
- 239000004033 plastic Substances 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- 230000008569 process Effects 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
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 description 3
- 239000004354 Hydroxyethyl cellulose Substances 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 238000010276 construction Methods 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
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 238000000655 nuclear magnetic resonance spectrum Methods 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 125000000542 sulfonic acid group Chemical group 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
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- 229920001938 Vegetable gum Polymers 0.000 description 2
- 230000001070 adhesive 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
- 239000006185 dispersion Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 150000002170 ethers Chemical group 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 230000010354 integration Effects 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
- 238000011056 performance test Methods 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 238000011160 research Methods 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 compound [Na+].[O-]S(=O)(=O)C=C BWYYYTVSBPRQCN-UHFFFAOYSA-M 0.000 description 2
- 239000007858 starting material Substances 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
- 239000002562 thickening agent Substances 0.000 description 2
- DZSVIVLGBJKQAP-UHFFFAOYSA-N 1-(2-methyl-5-propan-2-ylcyclohex-2-en-1-yl)propan-1-one Chemical compound CCC(=O)C1CC(C(C)C)CC=C1C DZSVIVLGBJKQAP-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
- 244000091691 Sesbania sesban Species 0.000 description 1
- 235000018287 Sesbania sesban Nutrition 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
- 230000000996 additive effect Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 239000012615 aggregate Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011083 cement mortar Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006266 etherification reaction Methods 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
- 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
- 239000004571 lime Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 125000001570 methylene group Chemical group [H]C([H])([*:1])[*:2] 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 230000003472 neutralizing effect Effects 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
- 239000011265 semifinished product Substances 0.000 description 1
- 229910021487 silica fume Inorganic materials 0.000 description 1
- TZLNJNUWVOGZJU-UHFFFAOYSA-M sodium;3-chloro-2-hydroxypropane-1-sulfonate Chemical compound [Na+].ClCC(O)CS([O-])(=O)=O TZLNJNUWVOGZJU-UHFFFAOYSA-M 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 125000001273 sulfonato group Chemical group [O-]S(*)(=O)=O 0.000 description 1
- 239000004094 surface-active agent Substances 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
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention provides sulfonated guar gum ether, a preparation method and application thereof. The sulfonated guar gum ether disclosed by the invention comprises the following raw materials in parts by weight: 100 parts of guar gum, 60-150 parts of water, 5-30 parts of sulfonation reagent, 5-30 parts of etherifying agent and 3-15 parts of catalyst; the sulfonating agent is 2-acrylamido-2-methylpropanesulfonic acid. The sulfonated guar gum ether disclosed by the invention has the advantages of 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, a preparation method and application thereof.
Background
The dry-mixed mortar belongs to commercial mortar, is initially called as premixed (dry) mortar in China according to the name of national standard GB/T25181-2019 premixed mortar, and is also called as dry powder, dry mixed material, dry powder mortar or dry mixed mortar, and is a mortar semi-finished product prepared by factory batching and mixing of cementing materials, mineral admixture, fine aggregate, additives and other solid materials, and does not contain mixing water. Dry-mixed mortar appeared in australia at the end of the 19 th century, and the european invention to mass production application of dry-mixed mortar has undergone over 50 years of history. Along with the continuous improvement of the requirements of the global building industry on the building technology, the building engineering has put higher requirements on the strength, the functionality, the durability and the like of the building mortar, and the development and the application of the dry-mixed mortar are gradually developed worldwide. Through the development of short time in China, the superiority of dry-mixed mortar in the aspects of quality, efficiency, economy, environmental protection and the like is increasingly displayed, and corresponding researches are gradually expanded.
The dry-mixed mortar consists of 3 main components such as cementing materials, aggregates, additives and the like. According to different purposes, the dry-mixed mortar with different functions can be prepared according to different formulas. The cementing material of the dry-mixed mortar mainly plays a cementing role, and comprises cement, lime, gypsum and the like; the aggregate mainly plays a role of a framework, and comprises sand, inert powder and the like; the additive mainly improves the workability and stability of mortar, has small addition amount and 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 the cement mortar, and is the most commonly used high molecular polymer, including Methyl Cellulose (MC), hydroxyethyl cellulose (HEC), hydroxyethyl methylcellulose (HEMC), hydroxypropyl methylcellulose (HPMC) and the like.
Guar ethers function in dry-mixed mortars to thicken and retain water, similar to cellulose ethers. It is a water-retaining and thickening material with high cost performance, and is used for replacing the cellulose ether with high cost.
CN102363637a discloses a preparation method and application of a thickening water-retaining agent for building dry-mixed mortar, 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 alkalization reaction at room temperature; (3) Adding etherifying agent for etherification under the pressure of 0.3-0.4MPa at 40-90 deg.c, preferably 50-70 deg.c for 2-5 hr, preferably 3-4 hr; (4) Cooling to 25-40 ℃, adding a neutralizing agent to the pH of the system to be 6-8, and collecting the thickening water-retaining agent from the reaction product. The thickening water-retaining agent for the building dry-mixed mortar can be applied to the building dry-mixed mortar to endow good water retention and workability; meanwhile, the price of the thickening water-retaining agent is obviously lower than that of cellulose ether, and the cost of the product formula can be obviously reduced by completely or partially replacing the cellulose ether.
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 reducer comprises, by weight, 1.0-1.5 parts of fly ash, 0.5-1.0 parts of air entraining agent, 0.2-0.8 parts of guar gum ether, 0.2-0.5 parts of water reducer and 0.2-0.5 parts of sulfonate, wherein the content of the fly ash is 1.0-1.5 parts of the diatomite water reducer is 1 part by weight. The mortar water-retaining thickener not only meets the requirements of water absorption, flame retardance, strength and the like, but also has the advantages of improving construction quality, avoiding wall cracks, along with simple preparation method, high operability, environmental friendliness and great 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, phosphorus slag, river sand, wood fiber, guar gum ether, a water reducing agent, an early strength agent and sodium nitrite; the cement comprises 15-25 parts by weight of river sand, 10-15 parts by weight of fly ash, 5-8 parts by weight of phosphorus slag, 3-6 parts by weight of wood fiber, 4-7 parts by weight of guar gum ether, 0.3-0.5 part by weight of water reducer, 0.5-0.8 part by weight of early strength agent and 1-3 parts by weight of sodium nitrite, relative to 100 parts by weight of river sand. The dry-mixed waterproof and antifreezing mortar can be used in a cold environment and has no cracking and peeling.
CN111908863a discloses a plastering mortar for a concrete wall surface of a plastic template and a preparation method thereof, silica fume, anti-cracking fiber, titanate, hydroxypropyl methylcellulose, hydroxypropyl guar gum ether, rubber powder and cement are added into water, and stirred to obtain the plastering mortar for the concrete wall surface of the plastic template; the raw materials are added in stages, so that the dispersibility of the inorganic components is improved, and as a mixture, the uniform dispersion of the components has an effect on the plastering performance of the mortar, the uniform and fine mortar is easy to smear, and the adhesive property after drying is good. The invention solves the problems of smoother molding surface, difficult adhesion of plastering, shortened construction period, reduced cost, driving the use of the plastic mold in the construction industry and solving the problem of low mortar adhesion strength of the existing plastic mold through the research of plastering technology.
CN103113486B discloses a sulfonic acid modified carboxymethyl hydroxypropyl guar gum, a preparation method and application thereof, wherein the structural formula of the sulfonic acid modified carboxymethyl hydroxypropyl guar gum is shown as follows:
wherein r=h, n=0, 1,2 or 3; or r=oh, n=0-6. The application is specifically used for preparing the fracturing fluid.
CN106146677a discloses a method for preparing dry-process sulfonic hydroxypropyl guar gum, which uses sodium 3-chloro-2-hydroxy propane sulfonate as sulfonating agent, wherein the sulfonic hydroxypropyl guar gum can be used as reinforcing agent, retention aid, filter aid and adhesive.
CN107522791B discloses a vegetable gum containing a sulfonic acid group, wherein the sulfonic acid group is located on any hydroxyl site of galactomannan and derivatives thereof, the galactomannan and derivatives thereof are selected from at least one of guar gum, coumarone, tianjiao, hydroxypropyl guar gum, carboxymethyl hydroxypropyl guar gum, hydroxypropyl coumarone, carboxymethyl coumarone and hydroxyethyl sesban gum, and the substitution degree of the sulfonic acid group is 0.20-0.80. The sulphonating agent is selected from oleum and/or sulphur trioxide. The vegetable gum containing the sulfonic group is used for preparing fracturing fluid.
However, the sulfonation reagent adopted in the preparation method has a severe reaction degree, is not easy to control, and has the water retention property of the prepared sulfonated guar gum ether to be further improved.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide the sulfonated guar gum ether, and the preparation method and the application thereof.
The invention aims to provide sulfonated guar gum ether, and the following technical scheme is adopted for achieving the purpose:
the sulfonated guar gum ether comprises the following raw materials in parts by weight:
the sulfonating agent is 2-acrylamido-2-methylpropanesulfonic acid.
The sulfonated guar gum ether disclosed by the invention uses water as a solvent, so that the production cost and the environmental protection pressure are greatly reduced; the usage amount of the etherifying agent and the sulfonating agent is less, the cost is low, the reaction requirement is reduced, the hydroxypropyl substitution degree of the sulfonated guar gum ether prepared by adopting 2-acrylamide-2-methylpropanesulfonic acid as the sulfonating agent ranges from 0.1 to 0.3, the sulfonate substitution degree ranges from 0.1 to 0.3, and the sulfonated guar gum ether belongs to a product with lower substitution degree, and has high viscosity and good water retention.
Specifically, the sulfonated guar gum ether comprises the following raw materials in parts by weight:
the weight parts of guar gum are 100 parts.
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 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, 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, or the like.
The catalyst is 3 to 15 parts by weight, for example, 3 parts, 4 parts, 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, 10 parts, 11 parts, 12 parts, 13 parts, 14 parts, 15 parts, or the like.
In the invention, the sulfonating agent is 2-acrylamido-2-methylpropanesulfonic acid. The 2-acrylamido-2-methylpropanesulfonic acid is adopted as the sulfonation reagent, and compared with other types of sulfonation reagents, the sulfonation reagent adopted by the invention has mild reaction and easily controlled reaction process.
In the invention, the etherifying agent is propylene oxide or ethylene oxide. Propylene oxide or ethylene oxide is adopted as an etherifying agent, so that compared with other types of etherifying agents, 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 ether of the invention is as follows:
the second purpose of the invention is to provide a preparation method of the sulfonated guar gum ether, which comprises the following steps:
mixing guar gum with water according to a proportion, adding a sulfonating reagent, an etherifying agent and a catalyst for reaction, cooling after the reaction is finished, adding acid for neutralization, and vacuum drying to obtain sulfonated guar gum ether.
Wherein the reaction time is 1-3 hours, for example 1 hour, 1.5 hours, 2 hours, 2.5 hours, 3 hours; the reaction temperature is 50-80 ℃, for example 50 ℃, 55 ℃, 60 ℃,65 ℃,70 ℃, 75 ℃ or 80 ℃, etc.
Wherein the temperature is 35-45deg.C, such as 35deg.C, 36deg.C, 37deg.C, 38deg.C, 39deg.C, 40deg.C, 41, 42, 43deg.C, 44 deg.C or 45deg.C.
Wherein acetic acid is adopted for neutralization by adding acid.
It is a further object of the present invention to provide the use of the sulfonated guar ether according to one of the objects for the preparation of dry-mixed mortars.
The invention further aims to provide dry-mixed mortar which comprises the sulfonated guar ether according to one of the aims, 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 weight percentage of the quartz sand is 50-70%, such as 50%, 51%, 52%, 53%, 54%, 55%, 56%, 57%, 58%, 59%, 60%, 61%, 62%, 63%, 64%, 65%, 66%, 67%, 68%, 69% or 70%, etc.
The weight percentage of the Portland cement is 30-40%, such as 30%, 31%, 32%, 33%, 34%, 35%, 36%, 37%, 38%, 39% or 40%, etc.
The weight percentage of the wood fiber 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 weight percentage of the sulfonated guar ether is 0.1-1%, such as 0.1%, 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 0.9% or 1%, etc.
The weight percentage of the dispersion rubber powder is 2-5%, such as 2%, 2.5%, 3%, 3.5%, 4%, 4.5% and 5%.
Compared with the prior art, the invention has the beneficial effects that:
the sulfonated guar gum ether disclosed by the invention uses water as a solvent, so that the production cost and the environmental protection pressure are greatly reduced; the etherifying agent and the sulfonating agent are less in use amount and low in cost, the reaction requirement is reduced, the hydroxypropyl substitution degree of the prepared sulfonated guar gum ether ranges from 0.1 to 0.3, the substitution degree of the sulfonic group ranges from 0.1 to 0.3, the sulfonated guar gum ether belongs to a product with lower substitution degree, the viscosity is high, the 2% solution viscosity is 25700-26100cp, the water retention property 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 resonance spectrum of a raw guar gum of the present invention;
FIG. 2 is a nuclear magnetic resonance spectrum of the sulfonated guar ether prepared by the invention;
fig. 3 is a nuclear magnetic resonance spectrum of the guar ether as a starting material of the present invention.
Detailed Description
The technical scheme of the invention is further described by the following specific embodiments.
The various starting materials of the present invention are commercially available, or may be prepared according to methods conventional in the art, unless specifically indicated.
Example 1
The preparation method of the sulfonated guar ether of the embodiment is as follows:
100 g of guar gum (nuclear magnetic hydrogen spectrum, see figure 1) was added to a small kneader, mixed with 90g of water, evacuated to remove air, charged with nitrogen, 12 g of sodium hydroxide, 20 g of 2-acrylamido-2-methylpropanesulfonic acid were added, the mixture was stirred for 15 minutes, then heated to 70 ℃ for 1 hour, 18 g of propylene oxide was added dropwise, and incubated at 70 ℃ for 1 hour, the mixture was cooled to room temperature, and neutralized to weakly alkaline by adding glacial acetic acid. And (3) vacuum drying the neutralized mixture, and crushing to obtain sulfonated guar ether sample A, wherein the nuclear magnetic hydrogen spectrum of the sulfonated guar ether sample A is shown in figure 2.
As can be seen from FIG. 2, the spectrum of hydrogen on the amide group-linked methylene group on the sulfonating agent was found to be 2.5ppm, the spectrum of hydrogen on the amide group-linked methyl group on the sulfonating agent was found to be 1.2ppm, the spectrum of methyl hydrogen on the etherifying agent was found to be 0.9ppm, and the degree of substitution by sulfonation was found to be 0.17 and the degree of substitution by hydroxypropyl was found to be 0.27 by integration of the peaks.
Viscosity test the viscosity of the 2% solution of sulfonated guar ether sample A prepared in this example was 26100cp at 25℃using a Brookfield viscometer (20 rpm).
Example 2
The preparation method of the sulfonated guar ether of the embodiment is as follows:
100 g guar gum and 80g water are added into a small kneader, the mixture is mixed with 80g water, the air is removed by vacuum pumping, nitrogen is filled, 10g sodium hydroxide and 15 g 2-acrylamido-2-methylpropanesulfonic acid are added, the mixture is stirred for 15 minutes, then the mixture is heated to 65 ℃ for 1 hour, 15 g propylene oxide is added dropwise, the temperature is kept at 65 ℃ for 1 hour, the mixture is cooled to room temperature, and the mixture is neutralized to alkalescence by adding glacial acetic acid. And (3) vacuum drying the neutralized mixture, and crushing to obtain the sulfonated guar gum ether sample B.
The sulfonated guar ether-like B prepared in this example had a sulfonation substitution of 0.12 and a hydroxypropyl substitution of 0.20, and a viscosity of 23200cp (Brookfield viscometer, 20 rpm) at 25℃in a 2% solution.
Comparative example 1
The preparation method of guar gum ether of the comparative example is as follows:
100 g guar gum and 110g water are added into a small kneader and mixed, air is removed by vacuum pumping, nitrogen is filled, 5 g sodium hydroxide is added, the mixture is stirred for 15 minutes, then, the mixture is heated to 70 ℃ for 1 hour, 18 g propylene oxide is added dropwise, the mixture is kept at 70 ℃ for 1 hour, the mixture is cooled to room temperature, and the mixture is neutralized to alkalescence by adding glacial acetic acid. And (3) vacuum drying the neutralized mixture, and crushing to obtain guar gum ether-like C, wherein the nuclear magnetic hydrogen spectrum of the guar gum ether-like C is shown in figure 3.
As can be seen from FIG. 3, the spectrum peak of methyl hydrogen as etherifying agent at 0.9ppm, and the hydroxypropyl substitution degree of guar gum ether-like C was calculated by integration of the peak to be 0.30.
Guar ether-like C had a viscosity of 26500cp (Brookfield viscometer, 20 rpm) at 25℃in a 2% solution.
Application example
Dry-mixed mortar is prepared by using the prepared sulfonated guar ether A, sulfonated guar ether B, guar ether C and commercial cellulose ether products HEC28000 as raw materials respectively, and the specific formulas are shown in table 1.
TABLE 1
And mixing the prepared dry-mixed mortar with 20% of water, filling the mixture into a test die, and testing and comparing the respective water retention rates W, wherein the water retention rates are tested according to JGJ/T70-2009 'building mortar basic performance test method Standard'. 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 dosage, and the sulfonated guar ether has the same excellent water retention effect as the commercial cellulose ether HEC 28000.
Example 3
This example differs from example 1 in that the etherifying agent is replaced by ethylene oxide, and the other is the same as in example 1.
Comparative example 2
This comparative example differs from example 1 in that the amount of sulfonation reagent used was 2 g, and the other was the same as in example 1.
Comparative example 3
This comparative example differs from example 1 in that the amount of sulphonating agent used is 50 g, all other things being equal to example 1.
Comparative example 4
This comparative example differs from example 1 in that the amount of etherifying agent used is 1 g, and the other is the same as in example 1.
Comparative example 5
This comparative example differs from example 1 in that the amount of etherifying agent used was 30 g, and the other is the same as in example 1.
Comparative example 6
This comparative example differs from example 1 in that the sulphonating agent is replaced by sodium vinylsulphonate, the remainder being identical to example 1.
Dry-mixed mortar was prepared from the sulfonated guar ethers prepared in example 3 and comparative examples 2 to 6 according to the formulation of table 1, and performance test was performed, and the test results are shown in table 3.
TABLE 3 Table 3
As can be seen from Table 3, example 1 uses 2-acrylamido-2-methylpropanesulfonic acid as the sulfonating agent, and has a high viscosity and better water retention than the sulfonated guar ether prepared in comparative example 6 using sodium vinylsulfonate as the sulfonating agent.
In example 1, propylene oxide is used as an etherifying agent, and compared with sulfonated guar gum ether prepared by using ethylene oxide as an etherifying agent in example 3, the sulfonated guar gum ether has better water retention rate.
The amount of the sulfonation agent of comparative example 2 used was too small, which resulted in a decrease in the water retention.
The amount of the sulfonation agent of comparative example 3 used was too large, which resulted in a decrease in viscosity and a decrease in water retention.
The amount of etherifying agent used in comparative example 4 was too small, and the water retention rate was lowered.
The use of too much etherifying agent in comparative example 5 lowers the viscosity and the water retention.
The detailed process equipment and process flow of the present invention are described by the above embodiments, but the present invention is not limited to, i.e., it does not mean that the present invention must be practiced depending on the detailed process equipment and process flow. It should be apparent to those skilled in the art that any modification of the present invention, equivalent substitution of raw materials for the product of the present invention, addition of auxiliary components, selection of specific modes, etc., falls within the scope of the present invention and the scope of disclosure.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited to the specific details of the above embodiments, and various simple modifications can be made to the technical solution of the present invention within the scope of the technical concept of the present invention, and all the simple modifications belong to the protection scope of the present invention.
In addition, the specific features described in the above embodiments may be combined in any suitable manner, and in order to avoid unnecessary repetition, various possible combinations are not described further.
Moreover, any combination of the various embodiments of the invention can be made without departing from the spirit of the invention, which should also be considered as disclosed herein.
Claims (5)
1. The dry-mixed mortar is characterized by comprising the following components in percentage by weight:
50-70% of quartz sand
Silicate cement 30-40%
0.1 to 1 percent of wood fiber
0.1 to 1 percent of sulfonated guar gum ether
2-5% of dispersed rubber powder, wherein the sum of the weight of the components is 100%;
the sulfonated guar gum ether comprises the following raw materials in parts by weight:
guar gum 100 parts
60-150 parts of water
5-30 parts of sulfonating reagent
5-18 parts of etherifying agent
3-15 parts of a catalyst;
the sulfonating reagent is 2-acrylamido-2-methylpropanesulfonic acid;
the etherifying agent is propylene oxide or ethylene oxide;
the catalyst is sodium hydroxide or potassium hydroxide.
2. The dry-mixed mortar of claim 1, wherein the preparation method of the sulfonated guar ether comprises the following steps:
mixing guar gum with water according to a proportion, adding a sulfonating reagent, an etherifying agent and a catalyst for reaction, cooling after the reaction is finished, adding acid for neutralization, and vacuum drying to obtain sulfonated guar gum ether.
3. Dry-mixed mortar according to claim 2, characterized in that the reaction time is 1-3 hours and the reaction temperature is 50-80 ℃.
4. A dry-mixed mortar according to claim 2, wherein the temperature of the cooling is 35-45 ℃.
5. Dry-mixed mortar according to claim 2, characterized in that the neutralization with acid is acetic acid.
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Citations (3)
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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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| Publication number | Priority date | Publication date | Assignee | Title |
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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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