CN1501957A - 吸水剂、其制备方法及其应用 - Google Patents
吸水剂、其制备方法及其应用 Download PDFInfo
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- CN1501957A CN1501957A CNA028038592A CN02803859A CN1501957A CN 1501957 A CN1501957 A CN 1501957A CN A028038592 A CNA028038592 A CN A028038592A CN 02803859 A CN02803859 A CN 02803859A CN 1501957 A CN1501957 A CN 1501957A
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- Prior art keywords
- water
- retaining agent
- polymkeric substance
- weight
- acid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000000034 method Methods 0.000 title claims description 17
- 239000006096 absorbing agent Substances 0.000 title abstract 2
- 238000004519 manufacturing process Methods 0.000 title description 3
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 59
- 229910001463 metal phosphate Inorganic materials 0.000 claims abstract description 32
- 229920000642 polymer Polymers 0.000 claims abstract description 15
- 239000002245 particle Substances 0.000 claims abstract description 13
- 238000010521 absorption reaction Methods 0.000 claims abstract description 4
- 239000000126 substance Substances 0.000 claims description 53
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 39
- 239000000178 monomer Substances 0.000 claims description 36
- 239000000203 mixture Substances 0.000 claims description 27
- 239000002250 absorbent Substances 0.000 claims description 25
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- 239000002253 acid Substances 0.000 claims description 11
- 230000011218 segmentation Effects 0.000 claims description 10
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- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 claims description 6
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- 239000004411 aluminium Substances 0.000 claims description 3
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- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims description 3
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- 239000010936 titanium Substances 0.000 claims description 3
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- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 3
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- 239000011701 zinc Substances 0.000 claims description 3
- 229910052726 zirconium Inorganic materials 0.000 claims description 3
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 claims description 2
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims 1
- 239000007788 liquid Substances 0.000 abstract description 4
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- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 12
- 239000001506 calcium phosphate Substances 0.000 description 12
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- NIXOWILDQLNWCW-UHFFFAOYSA-N Acrylic acid Chemical group OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 11
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- 239000012530 fluid Substances 0.000 description 9
- 150000002170 ethers Chemical class 0.000 description 8
- 229940052303 ethers for general anesthesia Drugs 0.000 description 8
- 125000000524 functional group Chemical group 0.000 description 8
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 8
- 238000003756 stirring Methods 0.000 description 8
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- 229910000389 calcium phosphate Inorganic materials 0.000 description 7
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- UWFRVQVNYNPBEF-UHFFFAOYSA-N 1-(2,4-dimethylphenyl)propan-1-one Chemical compound CCC(=O)C1=CC=C(C)C=C1C UWFRVQVNYNPBEF-UHFFFAOYSA-N 0.000 description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 6
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- 244000269722 Thea sinensis Species 0.000 description 5
- 230000002378 acidificating effect Effects 0.000 description 5
- 150000001298 alcohols Chemical class 0.000 description 5
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- 150000001412 amines Chemical class 0.000 description 5
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 5
- 229910052588 hydroxylapatite Inorganic materials 0.000 description 5
- 239000003999 initiator Substances 0.000 description 5
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 5
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- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 1
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/18—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing inorganic materials
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/42—Use of materials characterised by their function or physical properties
- A61L15/60—Liquid-swellable gel-forming materials, e.g. super-absorbents
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/013—Additives applied to the surface of polymers or polymer particles
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- Public Health (AREA)
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- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Absorbent Articles And Supports Therefor (AREA)
- Orthopedics, Nursing, And Contraception (AREA)
- Soil Conditioners And Soil-Stabilizing Materials (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
本发明涉及一种吸水剂，它含有其表面上结合有水不溶性金属磷酸盐的吸水剂聚合物粒子。该吸水剂具有包括高吸附能力、改善的液体传输性能和更快的膨胀速率在内的改进的性能分布。
Description
本发明涉及含有吸水剂聚合物粒子的吸水剂、其制备方法以及吸水剂用于吸收体液、生产卫生用品和用于改善土壤的用途。
吸水剂聚合物是已知的，也被称作形成水凝胶的聚合物或超强吸水剂聚合物(以下缩写为SAP)。它们是柔性的亲水性聚合物的网状结构，所述的亲水性聚合物在性质上可以是离子型的，也可以是非离子型的，它们能够通过形成水凝胶来吸收和结合含水流体。关于SAP、其用途及其生产的全面研究在F.L.Buchholz和A.T.Graham(编者)的“ModernSuperabsorbent Polymer Technology”，Wiley-VCH，纽约，1998中给出。
SAP尤其用于卫生用品诸如尿布、失禁护垫和短内裤、卫生巾等以吸收体液。在此经常存在的问题是超强吸水剂在流体的入口处膨胀至显著的程度并对随后的流体形成阻挡层。这阻止流体在吸水剂芯内的任何传输和分布。该超强吸水剂的现象被认为是凝胶阻塞。然后吸水剂芯再也不能吸收随后的液体量，因此不能控制流体在尿布表面的分布并且在极端情况下会出现泄漏。
DE-A-3 523 617、US-A-4,734,478和US-4,286,082记载了在混合物中含有二氧化硅的吸水剂树脂。据说加入的二氧化硅可以减小树脂的结块趋势。WO 87/00848记载了使用胶态载体物质诸如胶体二氧化硅来提高凝胶强度。
WO 95/11932公开了将细分的二氧化硅加入到表面后交联溶液中。EP-386 897公开了使用多价金属离子作为交联剂。将多价金属以其水溶性盐的形式使用。但是，所述吸水剂的性能分布并不是在每一方面都令人满意。
本发明的目的是提供具有改进的应用性能、特别是在压力下具有高吸收容量、改进的流体传输性能和较快的膨胀速率的吸水剂。
我们已发现，本发明的目的可以通过含有吸水剂聚合物颗粒的吸水剂来实现，所述的吸水剂聚合物的表面结合有水不溶性金属磷酸盐。
本发明还提供了制备前述权利要求中任何一项所述的吸水剂的方法，该方法包括：
a)将粒状吸水剂聚合物与细分的水不溶性金属磷酸盐紧密混合；或者
b)将细分的水不溶性金属磷酸盐的浆液涂覆到粒状吸水剂聚合物上；或者
c)在粒状吸水剂聚合物的存在下将含有磷酸盐离子的第一水溶液与第二水溶液接触，所述的第二溶液含有能形成水不溶性磷酸盐的金属的水溶性盐。
方便地讲，本发明的吸水剂的盐水流动传导率(SFC)一般为至少30×10-7cm3·s/g，负荷下的吸收能力(AUL)(0.7psi)为至少20g/g，离心保留能力(CRC)为至少24g/g。
将术语“结合”在最宽的意义上进行理解并且包括水不溶性金属磷酸盐和聚合物粒子表面之间的任何类型的相互作用。“结合”是指水不溶性金属磷酸盐实际上仅仅位于吸水剂聚合物粒子的表面上，并且仅仅以不明显的程度(如果有的话)进入粒子体内。通常将水不溶性金属磷酸盐通过物理相互作用、例如封闭在表面不规则处或靠近表面空隙中的形式结合。
有用的水不溶性金属磷酸盐还包括在技术意义上所谓的“磷酸盐”，可以认为是例如混合的磷酸盐氧化物、磷酸盐氢氧化物、磷酸盐硅酸盐、磷酸盐氟化物等。
优选的水不溶性金属磷酸盐是包括式M4P2O7、M2HPO4或M3PO4的磷酸盐的水不溶性金属磷酸盐，其中M是一种选自钙、镁、锶、钡、锌、铁、铝、钛、锆、铪、锡、铈、钪、钇和镧的金属或其混合物的等同物。M还可包括碱金属磷酸盐，只要混合的磷酸盐不溶于水即可。
优选的磷酸盐是磷酸氢钙、三代磷酸钙、磷灰石、式Ca5(PO4)[SiO4]的Thomas粉末、式AlPO4的块磷铝矿、式3CaNaPO4·VCa2SiO4的雷诺尼亚磷酸盐。特别优选的是三代磷酸钙、磷酸氢钙和磷灰石。术语“磷灰石”包括氟磷灰石、羟基磷灰石、氯磷灰石、碳酸盐磷灰石和碳酸盐氟磷灰石。可以理解，还可以使用各种水不溶性金属磷酸盐的混合物。
当将吸水剂用于卫生用品时，尤其可以考虑生理上安全的水不溶性金属磷酸盐及其混合物，诸如三代磷酸钙、羟基磷灰石或磷酸氢钙。
水不溶性金属磷酸盐的比例通常约为0.001-10重量％，优选0.01-5重量％，特别优选0.05-2.5重量％，基于吸水剂聚合物的重量计。
有用的吸水剂聚合物尤其是亲水性单体的聚合物、在适宜接枝基体上的一种或多种亲水性单体的接枝共聚物、交联的纤维素或淀粉醚、交联的羧甲基纤维素、部分交联的聚醚，或在含水流体中可膨胀的天然产物，诸如瓜耳胶衍生物、海藻和角叉菜胶。
适当的接枝基体可以是天然的或合成的原料。它们包括淀粉，天然淀粉，即选自玉米(玉蜀黍)淀粉、马铃薯淀粉、小麦淀粉、米淀粉、木薯淀粉、高梁淀粉、木薯淀粉、豌豆淀粉或其混合物；改性淀粉；淀粉的降解产物，例如氧化、酶催化或水解的淀粉；糊精例如焙烧的糊精，以及低级的低聚和多聚糖例如含有4-8元环的环糊精。有用的低聚和多聚糖还包括纤维素和淀粉和纤维素的衍生物。还可以使用聚乙烯醇、聚胺、聚酰胺、亲水性聚酯或聚亚烷基氧化物、特别是聚亚乙基氧化物和聚亚丙基氧化物。有用的聚亚烷基氧化物具有通式I
其中
R1、R2彼此独立地是氢；C1-C4-烷基；C2-C6-链烯基；芳基、特别是苯基；或(甲基)丙烯酰基；
X是氢或甲基，和
n是1-1000的整数，特别是10-400。
作为吸水剂聚合物，优选单烯属不饱和酸的聚合物。单烯属不饱和酸的聚合物优选至少部分地以它们的盐、特别是它们的碱金属盐诸如钠或钾盐或者铵盐的形式存在。该类聚合物尤其适于与含水流体接触时的凝胶。
特别优选单烯属不饱和C3-C6-羧酸和/或其碱金属盐或铵盐的交联吸水剂聚合物。尤其优选其中25-100％的酸基以碱金属盐或铵盐形式存在的交联聚丙烯酸。
该类聚合物例如可通过在交联剂的存在下聚合单烯属不饱和酸或其盐来得到。但是，也可以在没有交联剂的条件下进行聚合，随后进行交联。
吸水剂聚合物优选从以下物质聚合得到：
-49.9-99.9重量％的至少一种选自单烯属不饱和酸及其盐的单体A，
-0-50重量％、优选0-20重量％的至少一种不同于所述单体A的非交联的单烯属不饱和单体B，和
-0.001-20重量％、优选0.01-14重量％的至少一种交联单体C。
有用的单体A包括含有3-25个、优选3-6个碳原子的单烯属不饱和一元酸和二羧酸，它们还可用作盐或酸酐。例子是丙烯酸、甲基丙烯酸、乙基丙烯酸、α-氯代丙烯酸、巴豆酸、马来酸、马来酸酐、衣康酸、柠康酸、中康酸、戊烯二酸、乌头酸和富马酸。有用的单体A还包括含有4-10个、优选4-6个碳原子的单烯属不饱和二羧酸例如马来酸的单酯，诸如马来酸一甲酯。有用的单体A还包括单烯属不饱和的磺酸和膦酸，例如乙烯基磺酸、烯丙基磺酸、丙烯酸磺乙酯、甲基丙烯酸磺乙酯、丙烯酸磺丙酯、甲基丙烯酸磺丙酯、2-羟基-3-丙烯酰氧基丙基磺酸、2-羟基-3-甲基丙烯酰氧基丙基磺酸、苯乙烯磺酸、2-丙烯酰胺基-2-甲基丙磺酸、乙烯基膦酸和烯丙基膦酸以及它们的盐，特别是这些酸的钠盐、钾盐和铵盐。可以使用单体A本身或不同的单体A的混合物。规定的重量分数都按照酸的形式计。
优选的单体A是丙烯酸、甲基丙烯酸、乙烯基磺酸、2-丙烯酰胺基-2-甲基丙磺酸或其混合物。优选的单体A是丙烯酸和丙烯酸与其它的单体A的混合物，例如丙烯酸与甲基丙烯酸的混合物、丙烯酸与丙烯酰胺基丙磺酸的混合物或丙烯酸与乙烯基磺酸的混合物。特别优选丙烯酸是单体A的主要组成成分。
为了最优化本发明的聚合物的性能，明智的是使用不同于单体A的另外的单烯属不饱和单体B，因为它们不含酸基，但是它们可与单体A共聚并且是非交联的。这样的化合物包括例如单烯属不饱和腈类，诸如丙烯腈、甲基丙烯腈；上述单烯属不饱和羧酸的酰胺，例如丙烯酰胺、甲基丙烯酰胺；N-乙烯基酰胺，诸如N-乙烯基甲酰胺、N-乙烯基乙酰胺、N-甲基乙烯基乙酰胺、N-乙烯基吡咯烷酮和N-乙烯基己内酰胺。单体还包括饱和的C1-C4-羧酸的乙烯基酯，诸如甲酸乙烯酯、乙酸乙烯酯和丙酸乙烯酯；烷基中含有至少2个碳原子的烷基乙烯基醚，例如乙基乙烯基醚或丁基乙烯基醚；单烯属不饱和C3-C6-羧酸的酯，例如一元C1-C18-醇与丙烯酸、甲基丙烯酸或马来酸形成的酯，烷氧基化的一元饱和醇例如每摩尔醇与2-200摩尔环氧乙烷和/或环氧丙烷反应得到的含有10-25个碳原子的醇类的丙烯酸酯和甲基丙烯酸酯，以及聚乙二醇或聚丙二醇的单丙烯酸酯和单甲基丙烯酸酯，例如聚亚烷基二醇的摩尔质量(Mn)最大为2000。另外的适宜单体是苯乙烯和烷基取代的苯乙烯，诸如乙基苯乙烯或叔丁基苯乙烯。
单体B还可以以不同单体B的混合物、例如以任何比率组成的乙酸乙烯酯和丙烯酸2-羟基乙基酯的混合物形式使用。
有用的交联单体C包括分子内含有至少两个、例如2、3、4或5个烯属不饱和双键的化合物。该类化合物的例子是N，N’-亚甲基二-丙烯酰胺，均衍生自分子量为106-8500、优选400-2000的聚乙二醇的聚乙二醇二丙烯酸酯和聚乙二醇二甲基丙烯酸酯，三羟甲基丙烷三丙烯酸酯、三羟甲基丙烷三甲基丙烯酸酯、乙二醇二丙烯酸酯、乙二醇二甲基丙烯酸酯、丙二醇二丙烯酸酯、丙二醇二甲基丙烯酸酯、丁二醇二丙烯酸酯、丁二醇二甲基丙烯酸酯、己二醇二丙烯酸酯、己二醇二甲基丙烯酸酯、二甘醇二丙烯酸酯、二甘醇二甲基丙烯酸酯、三乙二醇二丙烯酸酯、三乙二醇二甲基丙烯酸酯、二丙二醇二丙烯酸酯、二丙二醇二甲基丙烯酸酯、三丙二醇二丙烯酸酯、三丙二醇二甲基丙烯酸酯、甲基丙烯酸烯丙酯，环氧乙烷和环氧丙烷的嵌段共聚物的二丙烯酸酯和二甲基丙烯酸酯，二-、三-、四-或五丙烯酸酯化或-甲基丙烯酸酯化的多元醇，诸如甘油、三羟甲基丙烷、季戊四醇或二季戊四醇，单烯属不饱和羧酸与烯属不饱和醇诸如烯丙醇、环己烯醇和二环戊烯基醇的酯，例如丙烯酸烯丙酯和甲基丙烯酸烯丙酯，以及三烯丙基胺，二烷基二烯丙基卤化铵，诸如二甲基二烯丙基氯化铵和二乙基二烯丙基氯化铵、四烯丙基乙二胺、二乙烯基苯、邻苯二甲酸二烯丙酯、分子量为106-4000的聚乙二醇的聚乙二醇二乙烯基醚、三羟甲基丙烷二烯丙基醚、丁二醇二乙烯基醚、季戊四醇三烯丙基醚、1摩尔乙二醇二缩水甘油醚或丙二醇二缩水甘油醚与2摩尔季戊四醇三烯丙基醚或烯丙醇的反应产物以及二乙烯基亚乙基脲。
优选水溶性的单体，即在20℃水中的溶解度至少为50g/l的化合物。这些化合物包括例如聚乙二醇二丙烯酸酯和聚乙二醇二甲基丙烯酸酯，2-400摩尔环氧乙烷与1摩尔二元醇或多元醇的加成产物的乙烯基醚，6-20摩尔环氧乙烷与1摩尔甘油的加成产物的乙二醇二丙烯酸酯、乙二醇二甲基丙烯酸酯或三丙烯酸酯和三甲基丙烯酸酯，季戊四醇三烯丙基醚和二乙烯基脲。
有用的单体C还包括含有至少一个烯属不饱和双键和至少一个在其活性方面与羧基互补的额外官能团的化合物。具有与羧基互补的活性的官能团包括例如羟基、氨基、环氧基团和氮丙啶基。使用的化合物包括例如上述单烯属不饱和羧酸的羟基烷基酯，诸如丙烯酸2-羟基乙基酯、丙烯酸3-羟基丙基酯、丙烯酸4-羟基丁基酯、(甲基)丙烯酸2-羟基乙基酯、(甲基)丙烯酸3-羟基丙基酯和(甲基)丙烯酸4-羟基丁基酯、烯丙基吡啶鎓盐溴化物，N-乙烯基咪唑，诸如N-乙烯基咪唑、1-乙烯基-2-甲基咪唑；和N-乙烯基咪唑啉，诸如N-乙烯基咪唑啉、1-乙烯基-2-甲基咪唑啉、1-乙烯基-2-乙基咪唑啉或1-乙烯基-2-丙基咪唑啉，在聚合过程中将它们以游离碱的形式、季铵化的形式或以盐的形式使用。还可以使用丙烯酸二甲基氨基乙基酯、甲基丙烯酸二甲基氨基乙基酯、丙烯酸二乙基氨基乙基酯或甲基丙烯酸二乙基氨基乙基酯。将这些基本的酯优选以季铵化的形式或以盐的形式使用。(甲基)丙烯酸缩水甘油酯也是有用的。
有用的交联单体C还包括含有至少两个在其活性方面能与聚合物的羧基互补的官能团的化合物。有用的官能团是异氰酸酯、酯和酰氨基以及上述官能团，诸如羟基、氨基、环氧基和氮丙啶基。有用的该类交联剂包括例如氨基醇类，诸如乙醇胺或三乙醇胺；二-和多元醇，诸如1，3-丁二醇、1，4-丁二醇、乙二醇、二甘醇、三乙二醇、四乙二醇、聚乙二醇、甘油、聚丙三醇、丙二醇、聚丙二醇、三羟甲基丙烷、季戊四醇、聚乙烯醇、山梨糖醇、淀粉，环氧乙烷和环氧丙烷的嵌段共聚物；多胺，诸如乙二胺、二亚乙基三胺、三亚乙基四胺、四亚乙基五胺、五亚乙基六胺和聚环乙亚胺，以及在所有情况下摩尔质量最大为4000000的聚胺；酯类，诸如失水山梨糖醇脂肪酸酯、乙氧基化的失水山梨糖醇脂肪酸酯；聚缩水甘油醚，诸如乙二醇二缩水甘油醚、聚乙二醇二缩水甘油醚、甘油二缩水甘油醚、甘油聚缩水甘油醚、二甘油聚缩水甘油醚、聚甘油聚缩水甘油醚、山梨糖醇聚缩水甘油醚、季戊四醇聚缩水甘油醚、丙二醇二缩水甘油醚和聚丙二醇二缩水甘油醚；多氮丙啶化合物，诸如2，2-二羟基甲基丁醇三[3-(1-氮丙啶基)丙酸酯；碳酸的二酰胺，诸如1，6-六亚甲基二亚乙基脲、二苯基甲烷二-4，4’-N，N’-二亚乙基脲；卤代环氧化合物，诸如表氯醇和α-甲基环氧氟丙烷；多异氰酸酯，诸如2，4-甲苯二异氰酸酯和六亚甲基二异氰酸酯；碳酸亚烷基酯，诸如1，3-二氧戊环-2-酮和4-甲基-1，3-二氧戊环-2-酮；以及二噁唑啉和噁唑烷酮，聚酰氨基胺及其与表氯醇的反应产物；以及聚季胺，诸如二甲胺与表氯醇的缩合产物，二烯丙基二甲基氯化铵的均聚物和共聚物，以及任选地被例如氯代甲烷季铵化的(甲基)丙烯酸二甲基氨基乙基酯的均聚物和共聚物。
吸水剂聚合物可以通过将单体A、B和C在水溶液中、任选地在适宜接枝基体的存在下进行自由基聚合来制得。聚合不仅可以在均匀水相中进行，而且可以是悬浮聚合的形式，在悬浮聚合的情况下单体的水溶液形成分散相。
在水溶液中的聚合优选以凝胶聚合的形式进行。它包括例如将被聚合的单体A、B和C的10-70重量％水溶液任选地在适宜接枝基体的存在下通过聚合引发剂利用Trommsdorff-Norrish效应进行聚合。
聚合通常在0-150℃、优选10-100℃的温度下进行，不仅可以在常压下进行，而且可以在高于大气压下或减压下进行。通常，聚合反应还可以在保护气氛、优选在氮气中进行。
用于制备这些产品的工业方法包括通常用于制备超强吸收剂的所有方法。适当的方法记载于例如“Modern Superabsorbent Polymer Technology”，F.L. Buchholz和A.T.Graham，Wiley-VCH，1998，第3章，在本文中将其引入作为参考。有用的聚合反应器包括常用的生产反应器、特别是溶液聚合情况下的带式反应器和捏合机(参见“Modern Superabsorbent PolymerTechnology”，第3.2.3节)。聚合物特别优选通过连续或间歇的捏合过程来制备。
适当的引发剂原则上包括一旦加热至聚合温度就能分解成自由基的所有化合物。聚合可以在光引发剂的存在下通过高能量辐射例如UV辐射的作用来引发。还可以通过电子束对可聚合的含水混合物的作用来引发聚合。
适当的引发剂包括例如过氧化合物，诸如有机过氧化物、有机氢过氧化物、过氧化氢、过硫酸盐、过硼酸盐、偶氮化合物和氧化还原催化剂。优选水溶性的引发剂。在某些情况下，优选使用不同的聚合引发剂的混合物，例如过氧化氢和过氧二硫酸钠或过氧二硫酸钾的混合物。有用的有机过氧化物包括例如乙酰丙酮过氧化物、甲基乙基酮过氧化物、叔丁基氢过氧化物、枯烯氢过氧化物、过新戊酸叔戊基酯、过新戊酸叔丁基酯、过新己酸叔丁基酯、过异丁酸叔丁基酯、过-2-乙基己酸叔丁基酯、过异壬酸叔丁基酯、过马来酸叔丁基酯、过苯甲酸叔丁基酯、二(2-乙基己基)过氧二碳酸酯、二环己基过氧二碳酸酯、二(4-叔丁基环己基)过氧二碳酸酯、二肉豆蔻基过氧二碳酸酯、二乙酰基过氧二碳酸酯、烯丙基过酸酯、过氧基新癸酸枯烯酯、过-3，5，5-三甲基己酸叔丁基酯、乙酰基环己基磺酰基过氧化物、二月桂基过氧化物、过氧化二苯甲酰和叔戊基过新癸酸酯。特别有用的聚合引发剂包括水溶性的偶氮引发剂，例如2，2’-偶氮二(2-脒基丙烷)二盐酸盐、2，2’-偶氮二(N，N’-二亚甲基)异丁脒二盐酸盐、2-(氨基甲酰基偶氮)异丁腈、2，2’-偶氮二[2-(2’-咪唑啉-2-基)丙烷]二盐酸盐和4，4’-偶氮二(4-氰基戊酸)。将提到的聚合引发剂以常用量例如以0.01-5重量％、优选0.05-2.0重量％的量使用，基于要被聚合物的单体计。
优选的氧化还原引发剂是水溶性引发剂并且包括作为氧化成分的至少一种上面详列的过氧化合物和作为还原成分的例如抗坏血酸、葡萄糖、山梨糖，铵或碱金属的亚硫酸盐、酸式亚硫酸盐、硫代硫酸盐、次亚硫酸盐、焦亚硫酸盐或硫化物，金属盐诸如铁(II)离子或羟基甲基次硫酸钠。在氧化还原催化剂中，还原成分优选为抗坏血酸或亚硫酸钠。例如，基于聚合中使用的单体的量计算，可以使用的氧化还原催化剂体系中含有3×10-6至1摩尔％的还原成分以及0.001-5.0摩尔％的氧化成分。
当利用高能量辐射引发聚合时，使用的引发剂通常是光引发剂。
将上述单烯属不饱和羧酸在有或没有单烯属不饱和共聚单体存在下聚合制备的并且分子量通常大于5000、优选大于50000的聚合物是通过将它们与含有至少两个对酸基呈反应性的基团的化合物发生反应来进行后交联。该反应可以在室温或者在最高至220℃的高温下进行。使用的交联剂是上述的单体C，单体C含有至少两个对于羧基具有互补反应性的官能团。
将用于后交联或凝胶交联的交联剂以0.5-20重量％、优选1-14重量％的量加入到形成的聚合物中，基于聚合物的量计算。
聚合后通常以水分含量为例如0-90重量％、通常是20-90重量％的水凝胶形式得到本发明的聚合物，通常利用已知方法首先将所述的水凝胶粗略地粉碎。水凝胶的粗略粉碎通过常用的撕裂和/或切割工具、例如在聚合物情况下在圆筒形反应器内通过排料泵的作用或者在带式聚合情况下通过切割轧辊或切割轧辊的组合来进行。
当未以中和形式使用单体A时，可以将得到的酸性聚合物调节至所需的中和程度，通常至少是25摩尔％、优选至少是50摩尔％、优选50-100摩尔％，基于酸官能团的单体单元计。另外，还可以在聚合之前或聚合过程中、例如在捏合机中调节中和的程度。
有用的中和剂包括碱金属的碱或氨/胺。优选使用氢氧化钠水溶液或氢氧化钾水溶液。但是，中和还可以利用碳酸钠、碳酸氢钠、碳酸钾或碳酸氢钾或其它的碳酸盐或碳酸氢盐或氨来进行。此外，伯、仲和叔胺也可用于中和。
随后将所得到的、优选(部分)中和的聚合物在升高的温度下、例如在80-250℃、特别是在100-180℃的温度下通过已知方法干燥(参见“ModernSuperabsorbent Polymer Technology”，第3.2.5节)。这样提供了(如果适当的话)进行数次研磨和分类操作以确定粒度的粉末或颗粒形式的聚合物(参见“Modern Superabsorbent Polymer Technology”，第3.2.6和3.2.7节)。
优选地，然后将得到的粒状聚合物进行表面后交联。为了进行表面后交联，将能与酸官能团反应的化合物优选以水溶液的形式涂覆到聚合物粒子的表面上。水溶液可含有与水混溶的有机溶剂。适当的溶剂是醇类诸如甲醇、乙醇、异丙醇或丙酮。
适当的后交联剂包括例如：
-二-或多缩水甘油基化合物，诸如膦酸二缩水甘油酯或乙二醇二缩水甘油醚、聚亚烷基二醇的二氯醇醚，
-烷氧基甲硅烷基化合物，
-基于聚醚或取代烃类的多氮丙啶、氮丙啶化合物，例如二-N-氮丙啶基甲烷，
-聚胺或聚酰氨基胺及其与表氯醇的反应产物，
-多元醇诸如乙二醇、1，2-丙二醇、1，4-丁二醇、甘油、甲基三甘醇、平均分子量Mw为200-10000的聚乙二醇、二-和聚甘油、季戊四醇、山梨糖醇、这些多元醇及其与羧酸或碳酸的酯诸如碳酸亚乙酯或碳酸亚丙酯的乙氧基化物，
-碳酸的衍生物诸如脲、硫脲、胍、双氰胺、2-噁唑烷酮及其衍生物、二噁唑啉、聚噁唑啉、二-和聚异氰酸酯，
-二-和多-N-羟甲基化合物，诸如亚甲基二(N-羟甲基甲基丙烯酰胺)或三聚氰胺-甲醛树脂，
-含有两个或多个嵌段异氰酸酯基团的化合物，例如被2，2，3，6-四甲基哌啶-4-酮封端的三甲基六亚甲基二异氰酸酯。
如果需要，还可以加入酸性催化剂例如对甲苯磺酸、磷酸、硼酸或磷酸二氢铵。
特别适当的后交联剂是二-或多缩水甘油基化合物，诸如乙二醇二缩水甘油醚，聚酰氨基胺与表氯醇的反应产物，和2-噁唑烷酮。
在常规的反应混合器或混合和干燥设备诸如Patterson-Kelly混合器、DRAIS湍流混合器、Ldige混合器、螺杆混合器、板式混合器、流化床混合器和Schugi-Mix中优选用交联剂的溶液进行喷涂来涂覆交联剂溶液。在交联剂溶液的喷涂之后是热处理步骤，优选在下游干燥器中在80-230℃、优选80-190℃、特别优选100-160℃下热处理5分钟至6小时、优选10分钟至2小时、特别优选10分钟至1小时，在该热处理过程中不仅可以取出裂解产物，而且可以除去溶剂级分。但是，通过加热夹套或吹入预热载气，干燥还可以在混合器本身中进行。
本发明的吸水剂通过用以干燥形式或以具有上述规定水分含量的粉碎水凝胶形式存在的粒状吸水剂聚合物作为原料并且将水不溶性金属磷酸盐涂覆到粒子表面上来制备。
为此，例如可以将粒状吸水剂聚合物与细分的水不溶性金属磷酸盐紧密混合。通常将细分的水不溶性金属磷酸盐在室温下加入到粒状吸水剂聚合物中并混合直到形成均匀的混合物。混合可以使用常规装置例如搅拌混合器、带式螺杆混合器或筒仓式螺杆混合器进行。与细分的水不溶性金属磷酸盐的混合可以在任何的表面后交联之前或之后进行，例如在涂覆后交联剂之后的热后处理过程中进行。
细分的水不溶性金属磷酸盐优选的平均粒度小于400μm、特别是小于100μm、更优选小于50μm、特别优选小于10μm、最优选为2-7μm。
另外，将细分的水不溶性金属磷酸盐的浆液涂覆到粒状吸水剂聚合物上。水不溶性金属磷酸盐的粒度优选如以上所规定的。将浆液例如通过喷涂进行涂覆。对于制备浆液，有用的分散介质包括：水，有机溶剂诸如醇类例如甲醇、乙醇、异丙醇，酮例如丙酮、甲基乙基酮，或水与上述有机溶剂的混合物。将浆液在常规的反应混合器或上述的混合和干燥系统中在室温至低于分散介质沸点的温度下、优选大约在室温下进行涂覆。适当的是，通过将细分的水不溶性金属磷酸盐分散于后交联剂的溶液中而将浆液的涂覆与表面后交联步骤相结合。另外，还可以在表面后交联步骤之前或之后涂覆浆液。在浆液的涂覆之后是干燥步骤。
在本发明的另一个实施方案中，通过在粒状吸水剂聚合物的存在下将含有磷酸盐离子的第一水溶液与第二水溶液接触而在吸水剂聚合物的表面上原位产生水不溶性金属磷酸盐，所述第二溶液含有能形成水不溶性磷酸盐的金属的水溶性盐。对于含有磷酸盐离子的溶液，抗衡离子优选为碱金属离子，诸如钠或钾离子。另外还可以将第一溶液用磷酸稀释。第二溶液含有至少一种能形成水不溶性磷酸盐的金属离子，诸如钙、镁、锶、钡、锌、铁、铝、钛、锆、铪、锡、铈、钪、钇或镧或其混合物的离子，优选钙的离子。它以足够水溶性盐的溶液形式，例如以卤化物诸如氯化物、溴化物、碘化物、氢氧化物、硫酸盐或硝酸盐的形式存在。作为超过其溶解度的结果，第一水溶液与第二水溶液一接触就会沉淀析出所需的水不溶性金属磷酸盐。在特别优选的实施方案中，将氯化钙溶液用作第一水溶液并且将一代、二代或三代磷酸钠溶液用作第二水溶液。原位形成三代磷酸钙并且它缓慢地转化呈羟基磷灰石。水不溶性金属磷酸盐在吸水剂聚合物表面上的原位沉淀可以在表面后处理之前、之中或之后进行。如果需要，可随后进行干燥步骤。
本发明的吸水剂可以用作水以及含水流体、特别是体液的吸收剂。可以将它们有益地用于生产卫生用品诸如尿布、失禁护垫和短内裤、棉塞或卫生巾。还可以将它们用于改善土壤，例如作为市场园林中的水分保留器。
以下实施例解释本发明。
I试验方法的描述
1、离心保留能力(CRC：离心保留能力)
该方法测定在茶袋中的形成水凝胶的聚合物的自由膨胀能力。将0.2000±0.0050g干燥聚合物(粒度分数为106-850μm)密封入尺寸为60×85mm的茶袋中。然后将茶袋在0.9重量％的盐溶液(至少0.83升盐水/1g聚合物粉末)中浸泡30分钟。然后将茶袋在250G下离心3分钟。通过将离心后的茶袋称重来确定吸收的液体量。
2、负荷下的吸收能力(AUL)(0.7psi)
用于确定AUL 0.7psi的测量装置是内径为60mm、高度为50mm的Plexiglas圆筒。粘接到其下侧的是筛孔尺寸为36μm的不锈钢筛网板。测量装置还包括直径为59mm的塑料板以及可与塑料板一起置于测量装置内的砝码。塑料板和砝码的总重为1345g。通过测定空Plexiglas圆筒和塑料板的重量并将其记录为W0来测定AUL 0.7psi。然后将0.900±0.005g形成凝胶的聚合物(粒度分布为106-800μm)称重加入Plexiglas圆筒内并在不锈钢筛网板上非常均匀地分布。然后将塑料板小心地置于Plexiglas圆筒内，将整个装置称重并将该重量记录为Wa。然后将砝码置于Plexiglas圆筒内的塑料板上。然后将直径为120mm、孔隙率为0的陶瓷过滤板置于直径为200mm、高度为30mm的陪替氏培养皿的中间并且将足量的0.9重量％氯化钠溶液引入到与塑料板表面齐平的液体表面上且没有润湿过滤板的表面。然后将直径为90mm、孔径＜20μm的圆形滤纸(S&S 589Schwarzband，来自Schleicher & Schll)置于陶瓷板上。然后将含有形成水凝胶的聚合物的Plexiglas圆筒和塑料板以及砝码一起放在滤纸上，将其放置60分钟。在该段时间的最后，从滤纸和陪替氏培养皿上移去整个装置，然后从Piexiglas圆筒中移去砝码。将含有溶胀的水凝胶的Plexiglas圆筒与塑料板一起称重并将该重量记录为Wb。
AUL通过如下方程式计算：
AUL 0.7psi[g/g]＝[Wb-Wa]/[Wa-W0]
3、盐水流动传导率(SFC)
用于测定SFC的试验方法记载于US 5,599,335。
4、膨胀速率(SR)
该方法在不存在限定压力的条件下测定水凝胶的初始膨胀能力。为了测定膨胀速率，将待测试的3.000±0.005g干燥水凝胶(水分含量＜5重量％)加入到直径为200mm、高度为100mm的18/10不锈钢软膏桶中并均匀分布到半圆形底部的中心。然后用分配器将60.0g的0.9重量％氯化钠溶液恰好加入至中心。得到在加入氯化钠溶液和最后一滴液体被水凝胶吸收之间的时间t(具有1/10秒刻度的停表)，以秒计算。通常是报道两次测定的平均值。
将膨胀速率(SR)按照如下方程式计算：
SR[g/g·s]＝吸收的盐溶液的量/(干燥水凝胶的量·吸附时间)
因此，膨胀速率表示每单位水凝胶在每秒钟内吸收的盐溶液的克数。
II制备实施例
实施例1
将容量至少为2.5升的玻璃瓶装上1kg的商购HySorbM7910型水凝胶(BASF AG，交联的聚丙烯酸钠)，然后加入0.5重量％的商购羟基磷灰石(由Budenheim销售)，首先将内含物粗略地预混合。所用的羟基磷灰石的平均粒度为3μm和5μm。然后玻璃瓶在辊式捏合机上滚动约30分钟。此后，混合物是均匀的。按照该方法得到的吸水剂的试验结果列在表1中。
表1
| 试验 | 平均粒度[μm] | CRC[g/g] | AUL 0.7psi[g/g] | SR[g/g·s] | SFC×10-7[cm3·s/g] |
| A(对照) | - | 28.0 | 23.0 | 0.14 | 41 |
| B+0.5％磷酸钙 | 5 | 29.0 | 23.6 | 0.20 | 58 |
| C+0.5％磷酸钙 | 3 | 29.9 | 24.4 | 0.25 | 70 |
实施例2
重复实施例1，所不同的是HySorbM7910型水凝胶被相同量的商购HySorbM7900型水凝胶(交联的聚丙烯酸钠)代替。所得到的吸水剂的试验结果列在表2中。
表2
| 试验 | 平均粒度[μm] | CRC[g/g] | AUL 0.7psi[g/g] | SR[g/g·s] | SFC×10-7[cm3·s/g] |
| D(对照) | - | 24.0 | 20.7 | 0.13 | 62 |
| E+0.5％磷酸钙 | 5 | 24.7 | 21.0 | 0.12 | 133 |
实施例3
重复实施例1，所不同的是使用不同量的平均粒度为5μm的三代磷酸钙。所得到的吸水剂的试验结果列在表3中。
表3
| 试验 | CRC[g/g] | AUL 0.7psi[g/g] | SFC×10-7[cm3·s/g] |
| F(对照) | 27.9 | 23.1 | 45 |
| G+0.1％磷酸钙 | 30.0 | 24.6 | 54 |
| H+0.2％磷酸钙 | 30.2 | 24.7 | 57 |
| I+0.4％磷酸钙 | 29.0 | 24.1 | 68 |
| J+0.8％磷酸钙 | 29.3 | 24.2 | 78 |
显然的是，将吸水剂聚合物用细分的三代磷酸钙进行表面处理可以增加离心保留能力、在负荷下的吸收能力以及盐水流动传导率。
实施例4
以下实施例解释说明水不溶性金属磷酸盐从悬浮液的涂覆。将结果报道在表4中。
实施例4.1(对比例)
将1500g的商购ASAP 403型超强吸水剂(BASF Corp.，Aberdeen)最初加入到Ldige实验室混合器中，然后利用双料喷嘴将75g异丙醇进行喷涂。此后，将得到的聚合物在干燥箱中干燥。
实施例4.2
将1500g的商购ASAP 403型超强吸水剂最初加入到Ldige实验室混合器中，然后利用双料喷嘴将通过搅拌已悬浮在75g异丙醇中的4.5g磷酸三钙(C13-09，SF，微细粉末，食品级-得自Chemische Fabrik Budenheim)进行喷涂。此后，将得到的聚合物在干燥箱中干燥。
实施例4.3
将1500g的商购ASAP 403型超强吸水剂最初加入到Ldige实验室混合器中，然后利用双料喷嘴将通过搅拌已悬浮在30g水中的4.5g磷酸三钙(C13-09，SF)进行喷涂。此后，将得到的粉末在干燥箱中干燥。
实施例4.4(对比例)
将1500g的商购ASAP 403型超强吸水剂最初加入到Ldige实验室混合器中，然后利用双料喷嘴将通过搅拌已悬浮在75g异丙醇中的4.5gSipernat 22 S型硅胶(购自Degussa)进行喷涂。此后，将得到的聚合物在干燥箱中干燥。
实施例4.5(对比例)
将1500g的商购ASAP 403型超强吸水剂最初加入到Ldige实验室混合器中，然后利用双料喷嘴将通过搅拌已悬浮在75g异丙醇中的4.5gSipernat D 17型硅胶(购自Degussa)进行喷涂。此后，将得到的聚合物在干燥箱中干燥。
实施例4.6(对比例)
将1500g的商购ASAP 500型超强吸水剂(BASF Corp.)最初加入到Ldige实验室混合器中，然后利用双料喷嘴将60g异丙醇进行喷涂。得到的聚合物不进行干燥。这是实施例4.7的对照样。
实施例4.7
将1500g的商购ASAP 403型超强吸水剂最初加入到Ldige实验室混合器中，然后利用双料喷嘴将通过搅拌已悬浮在60g异丙醇中的2.25g磷酸三钙(C13-09，SF)进行喷涂。得到的聚合物不进行干燥。
表4
| 实施例编号 | CRC[g/g] | AUL 0.7psi[g/g] | SFC×10-7[cm3·s/g] | QG[g/g·s] |
| 4.1* | 28.7 | 24.3 | 56 | 0.18 |
| 4.2 | 28.8 | 24.2 | 89 | 0.21 |
| 4.3 | 28.1 | 24.0 | 80 | 0.20 |
| 4.4* | 28.7 | 21.5 | 70 | 0.21 |
| 4.5* | 28.6 | 21.6 | 74 | 0.12 |
| 4.6* | 29.2 | 22.6 | 23 | --- |
| 4.7 | 29.5 | 22.9 | 31 | --- |
*对比例
实施例5
以下实施例解释说明在表面后交联的过程中水不溶性金属磷酸盐的应用。将结果报道在表5中(以5个测定值的平均值形式计算SFC)。
水凝胶的制备实施例
在40升的塑料桶中，通过搅拌加入氢氧化钠稀水溶液并通过换热器冷却，将6.9kg冰丙烯酸中和75摩尔％，然后用水稀释至30kg反应物质。通过搅拌将该溶液与50g聚乙二醇400二丙烯酸酯交联剂混合，并且通过通入氮气将密封的塑料桶惰性化。然后通过加入400mg过氧化氢和200mg抗坏血酸和10g过硫酸钠而开始聚合反应。反应结束后，将凝胶进行机械粉碎。然后将粉碎的凝胶在实验室的干燥箱中在150℃下干燥3小时，利用实验室的辊式捏合机进行研磨，最后筛分出200-850μm的粒度。这是在以下实施例中使用的基础聚合物。
实施例5.1(对比例)
利用双料喷嘴将Ldige犁式实验室混合器内的1200g基础聚合物用具有如下组成的后交联剂溶液进行喷涂：1.5重量％的异丙醇、3.5重量％的水、0.12重量％的2-噁唑烷酮，所有的百分数均基于使用的聚合物。随后将湿产物在175℃下在循环空气干燥箱中热处理60分钟。随后将干燥产物以850μm进行筛分以除去团块。
实施例5.2
将Ldige犁式实验室混合器内的1200g基础聚合物用具有如下组成的交联剂溶液进行喷涂：1.5重量％的异丙醇、3.5重量％的水、0.12重量％的2-噁唑烷酮、0.2重量％的磷酸三钙(C13-09，SF)，所有的百分数均基于使用的聚合物。然后将湿产物在175℃下在循环空气干燥箱中热处理60分钟。随后将干燥产物以850μm进行筛分以除去团块。
实施例5.3
将Ldige犁式实验室混合器内的1200g基础聚合物用具有如下组成的交联剂溶液进行喷涂：1.5重量％的异丙醇、3.5重量％的水、0.10重量％的乙二醇二缩水甘油醚、0.2重量％的磷酸三钙(C13-09，SF)，所有的百分数均基于使用的聚合物。然后将湿产物在150℃下在循环空气干燥箱中热处理60分钟。随后将干燥产物以850μm进行筛分以除去团块。
实施例5.4
在Waring犁式实验室混合器中将1200g基础聚合物首先与0.30重量％的粉状磷酸三钙(C13-09，SF)混合；然后用具有如下组成的交联剂溶液进行喷涂：1.5重量％的异丙醇、3.5重量％的水、0.10重量％的乙二醇二缩水甘油醚，所有的百分数均基于使用的聚合物。随后将湿产物在150℃下在循环空气干燥箱中热处理60分钟。随后将干燥产物以850μm进行筛分以除去团块。
表5
| 实施例编号 | CRC[g/g] | AUL 0.7psi[g/g] | SFC×10-7[cm3·s/g] |
| 5.1* | 31.0 | 24.5 | 18 |
| 5.2 | 30.9 | 24.7 | 32 |
| 5.3 | 31.7 | 24.9 | 34 |
| 5.4 | 31.5 | 25.0 | 29 |
*对比例
Claims (10)
1、一种吸水剂，含有其表面上结合有水不溶性金属磷酸盐的吸水剂聚合物粒子。
2、根据权利要求1所述的吸水剂，其中水不溶性金属磷酸盐是式M4P2O7、M2HPO4或M3PO4的磷酸盐，其中M是一种选自钙、镁、锶、钡、锌、铁、铝、钛、锆、铪、锡、铈、钪、钇和镧的金属或其混合物的等同物。
3、根据权利要求2所述的吸水剂，其中水不溶性金属磷酸盐选自磷酸氢钙、三代磷酸钙、磷灰石、雷诺尼亚磷酸盐、Thomas粉末、块磷铝矿及其混合物。
4、根据前述权利要求中任何一项所述的吸水剂，其中所述的吸水剂聚合物是从以下物质聚合得到的：
-49.9-99.9重量％的至少一种选自单烯属不饱和酸及其盐的单体A，
-0-50重量％的至少一种不同于所述单体A的单烯属不饱和单体B，和
-0.001-20重量％的至少一种交联单体C。
5、根据前述权利要求中任何一项所述的吸水剂，其中将所述的吸水剂聚合物进行表面后交联。
6、根据前述权利要求中任何一项所述的吸水剂，其中所述的水不溶性金属磷酸盐的比例是0.001-10重量％，基于所述吸水剂聚合物的重量计。
7、一种制备前述权利要求中任何一项所述吸水剂的方法，包括：
a)将粒状吸水剂聚合物与细分的水不溶性金属磷酸盐紧密混合；或者
b)将细分的水不溶性金属磷酸盐的浆液涂覆到粒状吸水剂聚合物上；或者
c)在粒状吸水剂聚合物的存在下将含有磷酸盐离子的第一水溶液与第二水溶液接触，所述的第二溶液含有能形成水不溶性磷酸盐的金属的水溶性盐。
8、根据权利要求7所述的方法，其中将所述粒状吸水剂聚合物在进行所述方法a)、b)或c)的同时或在其后进行表面后交联。
9、根据权利要求7或8所述的方法，其中所述的粒状吸水剂聚合物是水分含量为0-90重量％的粉碎的水凝胶形式。
10、权利要求1-6中任何一项所述的吸水剂用作体液的吸收剂、用于生产卫生用品或用于改善土壤的用途。
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| US (1) | US6831122B2 (zh) |
| EP (1) | EP1366111B2 (zh) |
| JP (1) | JP4991084B2 (zh) |
| CN (1) | CN1250622C (zh) |
| AT (1) | ATE552295T1 (zh) |
| AU (1) | AU2002250836A1 (zh) |
| WO (1) | WO2002060983A2 (zh) |
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2002
- 2002-01-18 US US10/250,826 patent/US6831122B2/en not_active Expired - Lifetime
- 2002-01-18 AU AU2002250836A patent/AU2002250836A1/en not_active Abandoned
- 2002-01-18 EP EP02719706.0A patent/EP1366111B2/de not_active Expired - Lifetime
- 2002-01-18 WO PCT/EP2002/000484 patent/WO2002060983A2/de active Application Filing
- 2002-01-18 AT AT02719706T patent/ATE552295T1/de active
- 2002-01-18 JP JP2002561546A patent/JP4991084B2/ja not_active Expired - Lifetime
- 2002-01-18 CN CNB028038592A patent/CN1250622C/zh not_active Expired - Lifetime
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101080245B (zh) * | 2004-10-20 | 2012-06-06 | 巴斯福股份公司 | 具有高流体输送和吸收能力的细粒状吸水性聚合物颗粒 |
| CN101489598B (zh) * | 2006-07-19 | 2015-07-08 | 巴斯夫欧洲公司 | 通过聚合单体溶液液滴生产具有较高渗透性的吸水性聚合物颗粒的方法 |
| CN101679648B (zh) * | 2007-03-23 | 2013-08-07 | 赢创斯托豪森有限责任公司 | 高渗透性高吸收性聚合物组合物 |
| CN106132534A (zh) * | 2014-03-31 | 2016-11-16 | 株式会社日本触媒 | 颗粒状吸水剂及其制造方法 |
| US10363544B2 (en) | 2014-03-31 | 2019-07-30 | Nippon Shokubai Co., Ltd. | Particulate water-absorbing agent |
| CN106132534B (zh) * | 2014-03-31 | 2020-06-19 | 株式会社日本触媒 | 颗粒状吸水剂及其制造方法 |
| CN107429162A (zh) * | 2015-04-06 | 2017-12-01 | Upl有限公司 | 吸水性组合物 |
| CN113717730A (zh) * | 2015-04-06 | 2021-11-30 | Upl 有限公司 | 吸水性组合物 |
| CN113717730B (zh) * | 2015-04-06 | 2023-09-29 | Upl 有限公司 | 吸水性组合物 |
Also Published As
| Publication number | Publication date |
|---|---|
| EP1366111A2 (de) | 2003-12-03 |
| CN1250622C (zh) | 2006-04-12 |
| JP4991084B2 (ja) | 2012-08-01 |
| JP2004517728A (ja) | 2004-06-17 |
| WO2002060983A3 (de) | 2002-11-07 |
| US20040077796A1 (en) | 2004-04-22 |
| EP1366111B2 (de) | 2020-04-29 |
| EP1366111B1 (de) | 2012-04-04 |
| US6831122B2 (en) | 2004-12-14 |
| ATE552295T1 (de) | 2012-04-15 |
| AU2002250836A1 (en) | 2002-08-12 |
| WO2002060983A2 (de) | 2002-08-08 |
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