CN116496020B - Method for reducing water absorption rate of phosphorus building gypsum, waterproofing agent used and preparation method - Google Patents
Method for reducing water absorption rate of phosphorus building gypsum, waterproofing agent used and preparation method Download PDFInfo
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- 239000010440 gypsum Substances 0.000 title claims abstract description 73
- 229910052602 gypsum Inorganic materials 0.000 title claims abstract description 73
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 31
- 238000004078 waterproofing Methods 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 22
- 238000010521 absorption reaction Methods 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title abstract description 29
- 239000011574 phosphorus Substances 0.000 title abstract description 29
- 229910052698 phosphorus Inorganic materials 0.000 title abstract description 29
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 23
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 23
- 235000021355 Stearic acid Nutrition 0.000 claims abstract description 18
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims abstract description 18
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000008117 stearic acid Substances 0.000 claims abstract description 18
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims abstract description 12
- 239000001110 calcium chloride Substances 0.000 claims abstract description 12
- 229910001628 calcium chloride Inorganic materials 0.000 claims abstract description 12
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 claims abstract description 12
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 claims abstract description 12
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 claims abstract description 12
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims abstract description 12
- 229920000053 polysorbate 80 Polymers 0.000 claims abstract description 12
- 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 claims abstract description 8
- 239000003054 catalyst Substances 0.000 claims abstract description 7
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 230000005540 biological transmission Effects 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims description 39
- PASHVRUKOFIRIK-UHFFFAOYSA-L calcium sulfate dihydrate Chemical compound O.O.[Ca+2].[O-]S([O-])(=O)=O PASHVRUKOFIRIK-UHFFFAOYSA-L 0.000 claims description 15
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 239000003513 alkali Substances 0.000 claims description 6
- 238000000576 coating method Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- -1 hydroxypropyl methylcellulose modified phosphogypsum Chemical class 0.000 claims description 4
- 239000011248 coating agent Substances 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 238000004132 cross linking Methods 0.000 claims description 2
- 238000004090 dissolution Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000000839 emulsion Substances 0.000 abstract description 11
- 230000000694 effects Effects 0.000 abstract description 2
- 238000005886 esterification reaction Methods 0.000 abstract description 2
- 230000002411 adverse Effects 0.000 abstract 1
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 239000004566 building material Substances 0.000 description 2
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 239000004568 cement Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 230000036571 hydration Effects 0.000 description 2
- 238000006703 hydration reaction Methods 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 239000012188 paraffin wax Substances 0.000 description 2
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 description 1
- 229920001807 Urea-formaldehyde Polymers 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- GZCGUPFRVQAUEE-SLPGGIOYSA-N aldehydo-D-glucose Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C=O GZCGUPFRVQAUEE-SLPGGIOYSA-N 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 229920003086 cellulose ether Polymers 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000001165 hydrophobic group Chemical group 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 150000003017 phosphorus Chemical class 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 230000002940 repellent Effects 0.000 description 1
- 239000005871 repellent Substances 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 description 1
- XYRAEZLPSATLHH-UHFFFAOYSA-N trisodium methoxy(trioxido)silane Chemical compound [Na+].[Na+].[Na+].CO[Si]([O-])([O-])[O-] XYRAEZLPSATLHH-UHFFFAOYSA-N 0.000 description 1
- 230000001755 vocal effect Effects 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/60—Agents for protection against chemical, physical or biological attack
- C04B2103/65—Water proofers or repellants
-
- 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
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Materials Applied To Surfaces To Minimize Adherence Of Mist Or Water (AREA)
Abstract
本发明提供降低磷建筑石膏吸水率的方法、采用的防水剂及制备方法，是以聚乙烯醇、硬脂酸、氯化钙为原料，以对甲基苯磺酸为催化剂，吐温80为乳化剂，通过聚乙烯醇与硬脂酸的酯化反应，制备成新型磷建筑石膏有机防水剂，将其外涂于石膏砌块表面可以形成一层致密的有机交联膜，阻碍水分子的进入。此外，通过内掺羟丙基甲基纤维素改性磷建筑石膏，进一步阻断石膏砌块中的水分子传输通道，降低吸水率。采用内掺协同外涂的方式能够使磷建筑石膏具有良好的防水性能。本发明不仅能提高磷建筑石膏的软化系数，还能降低有机乳液对其力学强度的不利影响，是一种高效的磷建筑石膏防水剂，能扩大磷建筑石膏在潮湿环境的使用范围。
The present invention provides a method for reducing the water absorption rate of phosphorus building gypsum, a waterproofing agent used and a preparation method. Polyvinyl alcohol, stearic acid and calcium chloride are used as raw materials, p-toluenesulfonic acid is used as a catalyst, and Tween 80 is used as an emulsifier. Through the esterification reaction of polyvinyl alcohol and stearic acid, a novel phosphorus building gypsum organic waterproofing agent is prepared. The novel phosphorus building gypsum organic waterproofing agent is applied to the surface of a gypsum block to form a dense organic cross-linked film to hinder the entry of water molecules. In addition, by internally adding hydroxypropyl methylcellulose to modify the phosphorus building gypsum, the water molecule transmission channel in the gypsum block is further blocked to reduce the water absorption rate. The internal addition and external application method can make the phosphorus building gypsum have good waterproof performance. The present invention can not only improve the softening coefficient of the phosphorus building gypsum, but also reduce the adverse effect of the organic emulsion on its mechanical strength. It is a highly efficient phosphorus building gypsum waterproofing agent and can expand the scope of use of the phosphorus building gypsum in a humid environment.
Description
技术领域Technical Field
本发明属于建筑材料领域，特别涉及一种降低磷建筑石膏吸水率的方法、采用的防水剂及制备方法。The invention belongs to the field of building materials, and particularly relates to a method for reducing the water absorption rate of phosphorus building gypsum, a used waterproofing agent and a preparation method.
背景技术Background technique
磷石膏是湿法磷酸产生的大宗工业固体废弃物，通过在一定温度下煅烧磷石膏制备建筑石膏是一种规模化消纳磷石膏的途径。建筑石膏制品可用于加工制备各类建筑材料，如室内抹灰、室内粉刷涂料、石膏板、石膏砌块等，具有轻质、保温隔热、防火和隔音性能好、绿色环保、成本低等优点。如郑州铁路职业技术学院申请的发明专利(公开号为CN109626937A)公开了一种防水建筑石膏板的制备方法，贵州大学申请的发明专利(公开号为CN110981385A)公开了一种轻质防潮磷建筑石膏砌块的制备方法。然而，耐水性能差、吸水率高、吸水后强度急剧降低等缺点限制了建筑石膏在潮湿环境中的使用，导致其使用范围有限。Phosphogypsum is a large industrial solid waste produced by wet phosphoric acid. The preparation of building gypsum by calcining phosphogypsum at a certain temperature is a way to dispose of phosphogypsum on a large scale. Building gypsum products can be used for processing and preparing various building materials, such as indoor plastering, indoor painting coatings, gypsum boards, gypsum blocks, etc., with the advantages of light weight, thermal insulation, good fire and sound insulation performance, green environmental protection, and low cost. For example, the invention patent applied by Zhengzhou Railway Vocational and Technical College (publication number CN109626937A) discloses a preparation method of a waterproof building gypsum board, and the invention patent applied by Guizhou University (publication number CN110981385A) discloses a preparation method of a lightweight moisture-proof phosphorus building gypsum block. However, the disadvantages of poor water resistance, high water absorption, and sharp decrease in strength after water absorption limit the use of building gypsum in humid environments, resulting in its limited scope of use.
近年来，为解决建筑石膏制品受潮后力学强度降低、易破裂变形等问题，通常采用以下措施：一是在石膏基复合胶凝材料外涂有机防水涂料提高耐水性能，如福建省万豪石膏工业有限公司的实用新型专利(公开号为CN210647156U)公开的一种防水的石膏制品；二是在建筑石膏内部掺入水泥矿化剂、火山岩等活性材料，提高石膏砌块的软化系数，如昆明理工大学的发明专利(公开号为CN106745144A)公开的一种复合矿化剂分解磷石膏的方法；三是在石膏中掺入水乳型防水剂如有机硅乳液、石蜡乳液等以改善石膏砌块的防水性能，如湖南省平江县城关石膏板厂的发明专利(CN86105530)公开了一种轻质、高强、耐水装饰石膏板。该板是在聚乙烯醇与石膏水化液中，再加入松香皂乳剂、半水石膏和脲醛树脂及石蜡乳液混合物均匀混合，然后成型、干燥而成。In recent years, in order to solve the problems of reduced mechanical strength, easy cracking and deformation of building gypsum products after being damp, the following measures are usually adopted: first, an organic waterproof coating is applied to the outside of the gypsum-based composite cementitious material to improve the water resistance, such as the utility model patent (publication number CN210647156U) of Fujian Wanhao Gypsum Industry Co., Ltd. discloses a waterproof gypsum product; second, active materials such as cement mineralizers and volcanic rocks are added to the building gypsum to improve the softening coefficient of gypsum blocks, such as the invention patent (publication number CN106745144A) of Kunming University of Science and Technology discloses a method for decomposing phosphogypsum with a composite mineralizer; third, a water-emulsion waterproofing agent such as silicone emulsion, paraffin emulsion, etc. is added to the gypsum to improve the waterproof performance of the gypsum blocks, such as the invention patent (CN86105530) of Chengguan Gypsum Board Factory, Pingjiang County, Hunan Province discloses a lightweight, high-strength, water-resistant decorative gypsum board. The board is made by adding rosin soap emulsion, semi-hydrated gypsum, urea-formaldehyde resin and paraffin emulsion into polyvinyl alcohol and gypsum hydration liquid, mixing them evenly, and then molding and drying them.
在以上三种技术措施中，第一种方法简单易行，但由于有机防水涂料裸露在石膏表面，易受水蚀影响，以至于脱落；第二种方法对建筑石膏的耐水性有明显提升，但是往往掺入矿物添加剂后，会使石膏砌块颜色发黑无光泽，限制硬制品使用范围；第三种方法内掺某一种或多种有机水乳液调控，能够保持石膏砌块的装饰效果，又能够达到防水的目的。然而，在建筑石膏内部掺入有机乳液，由于乳液的存在阻碍了硫酸钙晶体之间的相互粘结，虽然能降低建筑石膏的吸水率，但是会导致石膏砌块的力学强度降低。Among the above three technical measures, the first method is simple and easy to implement, but since the organic waterproof coating is exposed on the surface of the gypsum, it is easily affected by water erosion and even falls off; the second method significantly improves the water resistance of building gypsum, but after the addition of mineral additives, the gypsum blocks will become dark and dull, limiting the scope of use of hard products; the third method is to add one or more organic water emulsions to maintain the decorative effect of the gypsum blocks and achieve the purpose of waterproofing. However, when organic emulsions are added to the building gypsum, the presence of the emulsions hinders the mutual bonding between calcium sulfate crystals. Although it can reduce the water absorption rate of the building gypsum, it will lead to a decrease in the mechanical strength of the gypsum blocks.
因此，现有技术依然存在较大的问题，需要本领域技术人员提出创造性的改进方案。Therefore, there are still major problems with the prior art, and those skilled in the art are required to come up with creative improvement plans.
发明内容Summary of the invention
本发明提供了一种降低磷建筑石膏吸水率的方法、采用的防水剂及制备方法，以解决现有技术中存在的不足。The invention provides a method for reducing the water absorption rate of phosphorus building gypsum, a waterproofing agent used therein and a preparation method thereof, so as to solve the deficiencies existing in the prior art.
本发明是这样实现的：The present invention is achieved in that:
本发明首先提出了一种降低磷建筑石膏吸水率的方法，该方法包括对磷建筑石膏进行改性后用于浇筑石膏砌块，同时，采用一种磷建筑石膏有机防水剂将其外涂于石膏砌块表面形成一层有机交联膜，阻碍水分子的进入。而其中的改性磷建筑石膏是按重量份取0.15份羟丙基甲基纤维素掺入350份磷建筑石膏中，均匀搅拌后得羟丙基甲基纤维素改性磷建筑石膏粉用于浇筑石膏砌块。The present invention firstly proposes a method for reducing the water absorption rate of phosphorus building gypsum, which comprises modifying phosphorus building gypsum and using it for casting gypsum blocks, and at the same time, applying a phosphorus building gypsum organic waterproofing agent to the surface of the gypsum block to form an organic cross-linking film to prevent the entry of water molecules. The modified phosphorus building gypsum is prepared by adding 0.15 parts of hydroxypropyl methylcellulose to 350 parts of phosphorus building gypsum by weight, and uniformly stirring to obtain hydroxypropyl methylcellulose modified phosphorus building gypsum powder for casting gypsum blocks.
而在以上方案中，磷建筑石膏有机防水剂的制备组分至少包括聚乙烯醇、硬脂酸、氯化钙、对甲基苯磺酸和吐温80。在该防水剂的制备组分中，是以聚乙烯醇、硬脂酸、氯化钙作为原料，对甲基苯磺酸作为催化剂，吐温80作为乳化剂。In the above scheme, the preparation components of the phosphorus building gypsum organic waterproofing agent at least include polyvinyl alcohol, stearic acid, calcium chloride, p-toluenesulfonic acid and Tween 80. In the preparation components of the waterproofing agent, polyvinyl alcohol, stearic acid and calcium chloride are used as raw materials, p-toluenesulfonic acid is used as a catalyst, and Tween 80 is used as an emulsifier.
该磷建筑石膏有机防水剂的制备方法，至少包括如下步骤：The preparation method of the phosphorus building gypsum organic waterproofing agent comprises at least the following steps:
(1)按重量份将40份的氯化钙溶解于200份的去离子水中，加碱调节pH至8～10，并升温至95℃；(1) Dissolve 40 parts of calcium chloride in 200 parts of deionized water, add alkali to adjust the pH to 8-10, and heat to 95° C.;
(2)按重量份加入12～20份聚乙烯醇，并搅拌至完全溶解后保温0.3～0.5h；(2) adding 12 to 20 parts of polyvinyl alcohol by weight, stirring until completely dissolved and then keeping warm for 0.3 to 0.5 hours;
(3)按重量份加入2.4～6.4份硬脂酸，搅拌至完全溶解后加入1～3份对甲基苯磺酸后继续搅拌1～3h；(3) adding 2.4 to 6.4 parts of stearic acid by weight, stirring until completely dissolved, then adding 1 to 3 parts of p-toluenesulfonic acid and continuing to stir for 1 to 3 hours;
(4)降温至80℃，加入3～10份吐温80充分搅拌，自然冷却后得有机防水剂产品。(4) Cooling to 80°C, adding 3 to 10 parts of Tween 80 and stirring thoroughly, and cooling naturally to obtain an organic waterproofing agent product.
其中，步骤(1)中所述碱为氢氧化钠或氢氧化钾。步骤(1)中所述升温速度为5℃/min。步骤(2)中聚乙烯醇提前浸泡在去离子水中24h。步骤(2)的搅拌速度为2400r/min、搅拌时间为1～3h。步骤(3)中加入硬脂酸后的搅拌速度为2800r/min、搅拌时间为3h。步骤(3)中完全溶解指溶液由澄清变为乳白色。步骤(3)中加入对甲基苯磺酸后继续搅拌速度为2400r/min。步骤(4)中所述充分搅拌速度为3000r/min，搅拌时间0.1h。Wherein, the alkali described in step (1) is sodium hydroxide or potassium hydroxide. The heating rate described in step (1) is 5°C/min. In step (2), polyvinyl alcohol is soaked in deionized water for 24 hours in advance. The stirring speed of step (2) is 2400r/min and the stirring time is 1 to 3h. The stirring speed after adding stearic acid in step (3) is 2800r/min and the stirring time is 3h. Complete dissolution in step (3) means that the solution changes from clear to milky white. After adding p-toluenesulfonic acid in step (3), the stirring speed is continued at 2400r/min. The sufficient stirring speed described in step (4) is 3000r/min and the stirring time is 0.1h.
与现有技术相比，本发明取得了以下有益效果：在聚乙烯醇中加入金属盐可以提高增塑效率，以对甲基苯磺酸为催化剂促进了聚乙烯醇与硬脂酸的酯化反应，形成疏水基团RCOO-，添加乳化剂有助于药剂的乳化。将制备的有机防水剂外涂在磷建筑石膏砌块表面，乳液中的RCOO-会与石膏表面的Ca2+相互作用形成一层高分子有机交联膜，阻碍水分子的进入。此外，通过内掺羟丙基甲基纤维素，其分子中-OH能增强磷建筑石膏内部氢键的强度，有效阻断石膏砌块中的水分子传输通道，提高石膏砌块的防水性能。因此，外涂有机乳液与内掺纤维素醚能够提高石膏砌块的软化系数，降低砌块吸水率，增强磷建筑石膏的耐水性能，提高吸水后磷建筑石膏砌块的强度，且不影响石膏切块颜色。Compared with the prior art, the present invention has achieved the following beneficial effects: adding metal salt to polyvinyl alcohol can improve the plasticizing efficiency, using p-toluenesulfonic acid as a catalyst to promote the esterification reaction of polyvinyl alcohol and stearic acid to form a hydrophobic group RCOO-, and adding an emulsifier is helpful for the emulsification of the agent. The prepared organic waterproofing agent is applied externally on the surface of the phosphorus building gypsum block, and the RCOO- in the emulsion interacts with the Ca2 + on the surface of the gypsum to form a layer of high molecular organic cross-linked film, which hinders the entry of water molecules. In addition, by internally doping with hydroxypropyl methylcellulose, the -OH in its molecule can enhance the strength of the hydrogen bond inside the phosphorus building gypsum, effectively block the water molecule transmission channel in the gypsum block, and improve the waterproof performance of the gypsum block. Therefore, the external application of organic emulsion and the internal doping of cellulose ether can improve the softening coefficient of the gypsum block, reduce the water absorption rate of the block, enhance the water resistance of the phosphorus building gypsum, and improve the strength of the phosphorus building gypsum block after water absorption, and do not affect the color of the gypsum block.
附图说明BRIEF DESCRIPTION OF THE DRAWINGS
为了更清楚地说明本发明的实施例的技术方案，下面将对实施例的附图作简单地介绍。In order to more clearly illustrate the technical solution of the embodiment of the present invention, the drawings of the embodiment are briefly introduced below.
图1展示了一种有机防水剂产品；Figure 1 shows an organic water repellent product;
图2展示了外涂有机防水剂的磷建筑石膏砌块(浸泡后)。Figure 2 shows a phosphorus building gypsum block coated with an organic waterproofing agent (after immersion).
具体实施方式Detailed ways
下面结合实施例对本发明的实施方式作进一步详细描述。The embodiments of the present invention are further described in detail below with reference to the examples.
实施例1：Embodiment 1:
一种磷建筑石膏有机防水剂的制备及使用方法，以聚乙烯醇、硬脂酸、氯化钙为原料，以对甲基苯磺酸为催化剂，吐温80为乳化剂，制备有机防水剂，具体包括以下步骤：A preparation and use method of a phosphorus building gypsum organic waterproofing agent, using polyvinyl alcohol, stearic acid, and calcium chloride as raw materials, p-toluenesulfonic acid as a catalyst, and Tween 80 as an emulsifier to prepare the organic waterproofing agent, specifically comprising the following steps:
(1)按重量份将40份的氯化钙溶解与200份的去离子水中，加入碱调节pH至8，并升温至95℃；(2)在步骤(1)体系中，按重量份加入12份提前浸泡24h的聚乙烯醇，以2400r/min的速度搅拌1h待聚乙烯醇完全溶解后保温0.3h；(3)在步骤(2)体系中加入2.4份硬脂酸，以2800r/min的速度搅拌3h后，加入1份对甲基苯磺酸，并继续搅拌1h，温度为95℃；(4)待步骤(3)体系中温度降低至80℃后，按重量份加入3份吐温80，均匀搅拌0.1h，搅拌速度为3000r/min，自然冷却后得产品。(1) Dissolve 40 parts of calcium chloride by weight in 200 parts of deionized water, add alkali to adjust the pH to 8, and heat to 95°C; (2) Add 12 parts of polyvinyl alcohol soaked for 24 hours by weight to the system of step (1), stir at a speed of 2400 r/min for 1 hour until the polyvinyl alcohol is completely dissolved, and then keep warm for 0.3 hour; (3) Add 2.4 parts of stearic acid to the system of step (2), stir at a speed of 2800 r/min for 3 hours, add 1 part of p-toluenesulfonic acid, and continue stirring for 1 hour at a temperature of 95°C; (4) After the temperature in the system of step (3) drops to 80°C, add 3 parts of Tween 80 by weight, stir evenly for 0.1 hour at a stirring speed of 3000 r/min, and cool naturally to obtain the product.
实施例2：Embodiment 2:
一种磷建筑石膏有机防水剂的制备及使用方法，以聚乙烯醇、硬脂酸、氯化钙为原料，以对甲基苯磺酸为催化剂，吐温80为乳化剂，制备有机防水剂，具体包括以下步骤：A preparation and use method of a phosphorus building gypsum organic waterproofing agent, using polyvinyl alcohol, stearic acid, and calcium chloride as raw materials, p-toluenesulfonic acid as a catalyst, and Tween 80 as an emulsifier to prepare the organic waterproofing agent, specifically comprising the following steps:
(1)按重量份将40份的氯化钙溶解与200份的去离子水中，加入碱调节pH至9，并升温至95℃；(2)在步骤(1)体系中，按重量份加入16份提前浸泡24h的聚乙烯醇，以2400r/min的速度搅拌2h待聚乙烯醇完全溶解后保温0.4h；(3)在步骤(2)体系中加入3.2份硬脂酸，以2800r/min的速度搅拌3h后，加入2份对甲基苯磺酸，并继续搅拌2h，温度为95℃；(4)待步骤(3)体系中温度降低至80℃后，按重量份加入6份吐温80，均匀搅拌0.1h，搅拌速度为3000r/min，自然冷却后得产品。(1) Dissolve 40 parts of calcium chloride by weight in 200 parts of deionized water, add alkali to adjust the pH to 9, and heat to 95°C; (2) Add 16 parts of polyvinyl alcohol soaked for 24 hours by weight to the system of step (1), stir at a speed of 2400 r/min for 2 hours, and keep warm for 0.4 hours after the polyvinyl alcohol is completely dissolved; (3) Add 3.2 parts of stearic acid to the system of step (2), stir at a speed of 2800 r/min for 3 hours, add 2 parts of p-toluenesulfonic acid, and continue stirring for 2 hours at a temperature of 95°C; (4) After the temperature in the system of step (3) drops to 80°C, add 6 parts of Tween 80 by weight, stir evenly for 0.1 hour at a stirring speed of 3000 r/min, and cool naturally to obtain the product.
实施例3：Embodiment 3:
一种磷建筑石膏有机防水剂的制备及使用方法，以聚乙烯醇、硬脂酸、氯化钙为原料，以对甲基苯磺酸为催化剂，吐温80为乳化剂，制备有机防水剂，具体包括以下步骤：A preparation and use method of a phosphorus building gypsum organic waterproofing agent, using polyvinyl alcohol, stearic acid, and calcium chloride as raw materials, p-toluenesulfonic acid as a catalyst, and Tween 80 as an emulsifier to prepare the organic waterproofing agent, specifically comprising the following steps:
(1)按重量份将40份的氯化钙溶解与200份的去离子水中，加入碱调节pH至10，并升温至95℃；(2)在步骤(1)体系中，按重量份加入20份提前浸泡24h的聚乙烯醇，以2400r/min的速度搅拌3h待聚乙烯醇完全溶解后保温0.5h；(3)在步骤(2)体系中加入6.4份硬脂酸，以2800r/min的速度搅拌3h后，加入3份对甲基苯磺酸，并继续搅拌3h，温度为95℃；(4)待步骤(3)体系中温度降低至80℃后，按重量份加入10份吐温80，均匀搅拌0.1h，搅拌速度为3000r/min，自然冷却后得产品。(1) Dissolve 40 parts of calcium chloride by weight in 200 parts of deionized water, add alkali to adjust the pH to 10, and heat to 95°C; (2) Add 20 parts of polyvinyl alcohol soaked for 24 hours by weight to the system of step (1), stir at a speed of 2400 r/min for 3 hours, and keep warm for 0.5 hour after the polyvinyl alcohol is completely dissolved; (3) Add 6.4 parts of stearic acid to the system of step (2), stir at a speed of 2800 r/min for 3 hours, add 3 parts of p-toluenesulfonic acid, and continue stirring for 3 hours at a temperature of 95°C; (4) After the temperature in the system of step (3) drops to 80°C, add 10 parts of Tween 80 by weight, stir evenly for 0.1 hour at a stirring speed of 3000 r/min, and cool naturally to obtain the product.
将以上各实施例所制备的有机防水剂外涂于羟丙基甲基纤维素改性后的磷建筑石膏砌块表面，羟丙基甲基纤维素改性磷建筑石膏按重量份0.15份羟丙基甲基纤维素掺入350份磷建筑石膏中，均匀搅拌后得的羟丙基甲基纤维素改性磷建筑石膏粉，按水灰比0.55搅拌成料浆，倒入三联模中，水化硬化1d后，将制备好的有机防水剂均匀地涂抹在磷建筑石膏砌块表面，放置0.5h后，将石膏砌块完全浸泡在水中3d，取出后称重，并测试其力学强度。结果表明，经过内掺羟丙基甲基纤维素改性联同外涂新型有机防水剂的磷建筑石膏切块具有良好的耐水性能，吸水率降低至10.54％，软化系数达到0.81，相较目前单一有机防水剂(甲基硅酸钠0.69、聚乙烯醇为0.62、硬脂酸为0.74)有较明显的提高。The organic waterproofing agent prepared in the above embodiments is applied to the surface of the phosphorus building gypsum block modified with hydroxypropyl methylcellulose. 0.15 parts of hydroxypropyl methylcellulose by weight of the hydroxypropyl methylcellulose modified phosphorus building gypsum is added to 350 parts of the phosphorus building gypsum. The hydroxypropyl methylcellulose modified phosphorus building gypsum powder obtained after uniform stirring is stirred into a slurry at a water-cement ratio of 0.55, poured into a triple mold, and after hydration and hardening for 1 day, the prepared organic waterproofing agent is evenly applied to the surface of the phosphorus building gypsum block. After standing for 0.5h, the gypsum block is completely immersed in water for 3d, taken out and weighed, and its mechanical strength is tested. The results show that the phosphate building gypsum blocks modified with hydroxypropyl methylcellulose and coated with a new organic waterproofing agent have good water resistance, with the water absorption rate reduced to 10.54% and the softening coefficient reaching 0.81, which is significantly improved compared with the current single organic waterproofing agent (sodium methyl silicate 0.69, polyvinyl alcohol 0.62, stearic acid 0.74).
以上具体实施方式仅用以说明本发明的技术方案而非限制，尽管参照较佳实施例对本发明进行了详细说明，本领域的普通技术人员应当理解，可以对本发明的技术方案进行修改或者等同替换，而不脱离本发明技术方案的精神和范围，其均应涵盖在本发明的权利要求范围当中。The above specific implementation methods are only used to illustrate the technical solutions of the present invention rather than to limit it. Although the present invention has been described in detail with reference to the preferred embodiments, those skilled in the art should understand that the technical solutions of the present invention can be modified or replaced by equivalents without departing from the spirit and scope of the technical solutions of the present invention, which should be included in the scope of the claims of the present invention.
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