CN115340655A - Polyurethane material wiper strip material and application thereof - Google Patents

Polyurethane material wiper strip material and application thereof Download PDF

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Publication number
CN115340655A
CN115340655A CN202211018942.3A CN202211018942A CN115340655A CN 115340655 A CN115340655 A CN 115340655A CN 202211018942 A CN202211018942 A CN 202211018942A CN 115340655 A CN115340655 A CN 115340655A
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polyurethane
wiper strip
strip material
wiper
polyol
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CN115340655B (en
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唐凯荣
唐亮
任林
刘晶
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Midwest Shanghai Equipment Spare Parts Co ltd
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Midwest Shanghai Equipment Spare Parts Co ltd
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    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
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    • C08G18/12—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step using two or more compounds having active hydrogen in the first polymerisation step
    • A—HUMAN NECESSITIES
    • A47—FURNITURE; DOMESTIC ARTICLES OR APPLIANCES; COFFEE MILLS; SPICE MILLS; SUCTION CLEANERS IN GENERAL
    • A47L—DOMESTIC WASHING OR CLEANING; SUCTION CLEANERS IN GENERAL
    • A47L11/00—Machines for cleaning floors, carpets, furniture, walls, or wall coverings
    • A47L11/40—Parts or details of machines not provided for in groups A47L11/02 - A47L11/38, or not restricted to one of these groups, e.g. handles, arrangements of switches, skirts, buffers, levers
    • A47L11/4036—Parts or details of the surface treating tools
    • A47L11/4044—Vacuuming or pick-up tools; Squeegees
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    • C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
    • C08G18/4244—Polycondensates having carboxylic or carbonic ester groups in the main chain containing oxygen in the form of ether groups
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    • C08G18/6607—Compounds of groups C08G18/42, C08G18/48, or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3203
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    • C08G18/751—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring
    • C08G18/752—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group
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Abstract

The invention discloses a polyurethane wiper strip material and application thereof, and relates to the technical field of floor cleaning machine wiper strip materials, in particular to the field of preparation of a polyurethane material composition. The polyurethane wiper strip material comprises the components of a polyol composition, isocyanate, a chain extender, a modified nano metal oxide and a functional additive. Wherein the polyol composition comprises polyether polyol, polyester polyol, alkyl hydroxyl polysiloxane and hydroxyl-terminated polybutadiene; the functional additive comprises an antioxidant, silver powder and an ultraviolet absorber. The polyurethane material wiper rubber strip obtained through the prepolymer two-step process and vulcanization of the components has the advantages of low hardness, high resilience, mildew resistance, antibiosis and yellowing resistance, and meanwhile has excellent wear resistance and wiper working performance, and can be applied to wiper accessories of a floor washing machine.

Description

Polyurethane material wiper strip material and application thereof
Technical Field
The invention relates to the technical field of floor cleaning machine wiper strip materials, in particular to the field of preparation of a polyurethane material composition.
Background
Under the background of fast pace of modern life, the traditional mode of cleaning the ground by the manual mop has low efficiency and high cost, and has larger physical labor burden for workers. The cleaning mode of the floor cleaning machine is faster and more effective, and the floor cleaning machine is particularly suitable for cleaning large-area hard floors and does not need workers to pay excessive physical labor.
The floor washing machine is also called a ground washing machine and a floor washing and drying machine, and the floor washing machine replaces manpower for cleaning through machinery. The cleaning device can clean the hard ground, can treat sewage generated after cleaning by using the water wiping rubber strip and the water absorbing rake, and is widely applied to places with wide hard ground, such as large supermarkets, markets, docks, airports, workshops, warehouses, schools, hospitals, restaurants, stores and the like. The water wiping rubber strip is used as a water wiping part, is easy to wear due to long-time contact friction with a hard ground, is easy to mildew, yellow and crack and damage in a severe environment with partial heavy oil stains, directly reduces the water wiping effect of the water wiping rubber strip on the hard ground after being worn, and even causes the residual of sewage, thereby affecting the cleanliness of the ground.
At present, the wiper strips on the market can be divided into two categories of rubber and polyurethane according to the material. The water wiping rubber strip made of common natural rubber has good elasticity, is suitable for smooth ground environments such as markets, offices and the like, has relatively low price, but has the defects of no oil resistance, quick abrasion, incomplete sewage recovery and short service life. In order to reduce the degree of friction and increase the wear resistance of the wiper strip, there are disclosed modification methods of rubber, physical treatments such as impregnation, lamination, kneading of a lubricant and a resin, and chemical treatments of various drugs such as acids, bases, halogens, and the like. Among them, halogen treatment such as chlorination treatment is common. However, the initial friction coefficient can be reduced by the chlorination treatment, but the increase in friction coefficient and the deterioration of the sliding property are caused by the long-term use. In addition, wiper strips made from synthetic rubbers having a saturated polymer chain structure, such as ethylene-propylene-diene rubber (EPDM), have surfaces which cannot be hardened by halogenation due to the saturated polymer chain.
The polyurethane wiping strip is low in hardness, and has excellent performances of tear resistance, acid and alkali resistance, oil resistance, strong wiping property, low possibility of abrasion and the like. Among them, some one-component polyether or polyester type polyurethane wiper strips have excellent mechanical strength and elasticity, very good adhesion and abrasion resistance, and a simple process of extrusion from a melt, but have yet to be improved in uv resistance, yellowing resistance, weather resistance, and low-temperature resilience.
Disclosure of Invention
In order to solve the problems in the prior art, the invention discloses a polyurethane material wiper strip material with low hardness, high resilience and good wiping effect and application thereof, and the technical scheme is as follows:
the polyurethane wiper strip material comprises the raw materials of a polyol composition, a polyisocyanate composition, a chain extender, a modified nano metal oxide and a functional additive; wherein the polyol composition comprises polyether polyol, polyester polyol, alkyl hydroxyl polysiloxane and hydroxyl-terminated polybutadiene; the chain extender is 1, 4-Butanediol (BDO) or 1, 6-Hexanediol (HDO); the functional additive comprises an antioxidant, silver powder and an ultraviolet absorber.
As a further scheme of the invention, the polyether polyol is one or more of polyoxypropylene-polyoxyethylene glycol with the number average molecular weight of 500-3000g/mol and polytetrahydrofuran ether glycol (PTMG). "xx-hydroxyl polyether polyols" are to be understood as being nominally xx-hydroxyl polyether polyols. In practice, the nominal hydroxyl number (number of hydroxyl groups) deviates because of the various side reactions during the polyol synthesis which lead to hydroxyl group contents which are actually below the nominal assumption. Polyether polyol as a 'soft segment' unit in a polyurethane wiper strip material has a main influence on the rebound resilience and the water resistance of the wiper strip material, because when the hardness of a polyurethane elastomer is close, the rebound resilience of a polyether soft segment is higher than that of a polyester soft segment, and the fundamental reason is that the space bit group of ether groups in polyether is small and the softness of a molecular chain segment is good. While polyoxypropylene-polyoxyethylene glycols and polytetrahydrofuran ether glycol (PTMG) are typical polyether glycols, the segments are quite soft. It is known to those skilled in the art that as the relative molecular mass of the soft segment increases, the resilience of the polyurethane increases accordingly, because as the relative molecular mass increases, the number of conformations of the molecules increases, and the flexibility of the molecular chain increases. However, when the relative molecular weight exceeds 3000, the rebound resilience of the polyurethane is more directly related to the soft segment content, and too high a soft segment molecular weight easily causes a decrease in hardness and abrasion resistance of the polyurethane wiper strip.
As a further aspect of the present invention, the polyester polyol is prepared as follows: vacuumizing a reaction kettle, introducing nitrogen, and sequentially adding phthalic anhydride, diethylene glycol, 1, 6-hexanediol, trimethylolpropane and a catalyst into the reaction kettle, wherein the weight ratio of phthalic anhydride: diethylene glycol: 1, 6-hexanediol: trimethylolpropane = 51-54. Stirring, heating to 140-150 deg.C, maintaining for 1-3h, removing water generated during melt polycondensation, heating to 170-180 deg.C, maintaining for 6-10h, and detecting acid value below 3mg KOH/g. The polyester polyol is formed by carrying out melt polycondensation on dicarboxylic anhydride, dihydric alcohol and polyhydric alcohol in a reaction kettle under a nitrogen atmosphere. As known to those skilled in the art, the nitrogen gas is always kept in the reaction kettle, and the two main functions are to eliminate the residual oxygen in the reaction system to avoid color deepening, and to take out the moisture generated by the reaction, thereby promoting the polymerization reaction to proceed to the expected direction. In addition, phthalic anhydride provides a hard polyester segment due to certain structural rigidity, so that the final product has certain hardness and wear resistance, and diethylene glycol, 1, 6-hexanediol and trimethylolpropane have longer carbon chains, so that a soft polyester segment can be provided. The soft-hard segmented polyester structure is beneficial to forming a microphase separation structure of polyurethane, and the comprehensive mechanical property, the coordination modulus and the resilience of the material are improved. Furthermore, it is known to the person skilled in the art that the catalysts used for the polycondensation are generally organometallic compounds, in particular of tin, zinc, bismuth, titanium, zirconium, aluminum. For example tin (II) salts of organic carboxylic acids, such catalysts being tin (II) acetate, tin (II) octoate and tin (II) laurate, and the dialkyltin (IV) salts of organic carboxylic acids, such catalysts being dibutyltin diacetate and dibutyltin dilaurate. The catalyst used in the preparation process of the polyester polyol is monobutyl tin oxide.
As a further embodiment of the present invention, the structural formula of the alkylhydroxy polysiloxane is as follows:
Figure BDA0003813310660000031
wherein n is an integer between 5 and 20, and a + b is an integer between 4 and 10.
The introduction of the alkyl hydroxyl polysiloxane is mainly used for further improving the ultraviolet resistance, yellowing resistance, weather resistance and low-temperature resilience of the polyurethane material wiper strip. The silicon-methyl structure in the polysiloxane increases the distance between molecules, so that the macromolecular chain is easy to orient along the acting force direction, the submicroscopic phase separation of soft and hard chain segments is strengthened, the structural regularity and the tensile strength of the material in an aggregation state are improved, and the tensile elongation is increased. However, when the value of n of the polysiloxane segment unit is too large (exceeding 20), the mechanical properties, particularly tensile strength, of the polyurethane wiper strip material are significantly impaired, and the transparency of the polyurethane wiper strip material is affected due to an increased degree of microphase separation caused by further incompatibility of the polysiloxane and the polyether/polyester segment.
The alkylhydroxy polysiloxane can be directly purchased from products with corresponding specifications on the market, such as Corning.Co, wacker chemical (Wacker.Co), chongyao science and technology and other companies, and can also be manufactured by self. As is familiar to those skilled in the art, the self-made method is generally that hydrogen terminated silicone oil and allyl polyether are subjected to hydrosilylation addition reaction under the action of a platinum catalyst.
As a further embodiment of the invention, the hydroxyl-terminated polybutadiene (HTPB) has a data molecular weight of 2000 to 4000g/mol. Polybutadiene is introduced into a polyurethane chain segment as a soft segment structural unit, has excellent hydrolysis resistance, low-temperature resilience and corrosion resistance, and can be copolymerized with a hard polyisocyanate segment together with other polyether, polyester and polysiloxane soft segments to improve the thermodynamic incompatibility of the soft segment and the hard segment and form a morphological structure with two spontaneous micro-phase separation, so that the mechanical property of the polyurethane material is comprehensively improved. The hydroxyl-terminated polybutadiene can be directly purchased from products with corresponding specifications on the market, such as Riming chemical engineering Co., ltd., germany ARCO, japan Caoda corporation and the like
In a further embodiment of the invention, the isocyanate is an aliphatic diisocyanate, more preferably Hexamethylene Diisocyanate (HDI) or isophorone diisocyanate (IPDI). HDI and IPDI have better rebound resilience and yellowing resistance than aromatic isocyanates such as Toluene Diisocyanate (TDI) and diphenylmethane diisocyanate (MDI).
As a further scheme of the invention, the modified nano metal oxide is nano SiO subjected to surface treatment by using a silane coupling agent 2 Or nano Al 2 O 3 Adding intoThe addition amount is 0.5-2.0% of the total material mass fraction. The nano metal oxide is a material with a tiny particle size and a large specific surface area, and the thermal stability and the aging resistance of the material can be improved by adding the nano metal oxide into polyurethane, and particularly the wear resistance of the material is improved. Nano SiO 2 Or nano Al 2 O 3 The surface has a large number of active groups of hydroxyl groups, and the hydroxyl groups can be combined with the main polyurethane structure through van der Waals force or covalent bonds. However, such nanoparticles have a high specific surface energy, cannot be uniformly dispersed in polyurethane, and reduce the compatibility of a mixed system, and therefore, it is necessary to further improve the dispersibility of the nano metal oxide by means of, for example, surface modification.
The preparation method of the modified nano metal oxide comprises the following steps: taking nano SiO 2 Or nano Al 2 O 3 Drying, cooling to room temperature, placing in a reaction kettle, adding a silane coupling agent solution diluted by absolute ethyl alcohol, performing ultrasonic dispersion and stirring, taking out, and drying to obtain the surface modified nano metal oxide. The silane coupling agent is preferably one or more of Aminopropyltriethoxysilane (APTES), 3-glycidoxypropyltrimethoxysilane, gamma-aminopropylmethyldiethoxysilane and methyltrimethoxysilane.
As a further embodiment of the present invention, in the functional additive, the antioxidant is a common commercially available product, namely antioxidant 1010. The antioxidant is hindered phenol, has good compatibility with polyurethane materials, and effectively slows down the oxidation of the polyurethane material wiper strip so as to improve the yellowing resistance, and the skilled in the art knows that the higher the addition of the antioxidant is, the better the yellowing resistance is, but the excessive antioxidant does not further improve the yellowing resistance, increases the raw material cost and influences the mechanical property of the polyurethane material wiper strip, so that the addition of the antioxidant is 0.1-0.5%. The ultraviolet absorbent is a composition of benzotriazole 1130 ultraviolet absorbent and hindered amine 292 light stabilizer, and the addition amounts of the ultraviolet absorbent and the hindered amine 292 light stabilizer are respectively 0.5-2.0% and 0.1-0.5% of the mass fraction of the total material. The 1130 UV absorber is a hydroxyphenylbenzotriazole UV absorber, used in combination with a Hindered amine 292 light stabilizer (HALS). The common synergist can obviously improve the performance of the polyurethane wiper strip and prevent the polyurethane wiper strip from losing luster, cracking, foaming, falling off and discoloring. The UV absorbers are commercially available in the corresponding specifications, such as Tinuvin1130 and Tinuvin292 from BASF, germany. The addition amount of the silver powder is 0.2-0.5% of the total material mass fraction, and the main function of the silver powder is antibacterial, bactericidal and/or durability enhancing activity.
As a further aspect of the present invention, the preparation method of the polyurethane wiper strip material includes the following steps:
(A) Preparing a polyurethane prepolymer: weighing the polyol composition according to a proportion, carrying out vacuum dehydration at the temperature of 100-110 ℃ under the negative pressure of-0.09 to-0.1 MPa, cooling to the temperature below 70 ℃ after the water content is lower than 0.05 percent, adding isocyanate, heating to the temperature of 85-95 ℃ for reaction, cooling to the temperature below 60 ℃ after the content of isocyanate groups (-NCO) reaches the theoretical end value, and carrying out vacuum defoaming to obtain a polyurethane prepolymer which is sealed and stored for later use.
(B) Chain extension and vulcanization: heating the polyurethane prepolymer to 80-85 ℃, adding the modified nano metal oxide, the antioxidant, the silver powder and the ultraviolet absorber, uniformly stirring, adding the measured chain extender, rapidly stirring, pouring into a preheated flat plate mold coated with a release agent after vacuum defoaming, demolding after pressurization vulcanization is carried out for 10-30min at 110-120 ℃ when the gel point is reached, and vulcanizing at 100-120 ℃ for 16-20h to obtain the polyurethane wiping strip material.
As a further scheme of the invention, the polyurethane wiper strip material has the advantages of low hardness, high resilience, mildew resistance, antibiosis and yellowing resistance, and meanwhile has excellent wear resistance and wiper working performance, and can be applied to wiper accessories of a floor washing machine.
The technical scheme provided by the embodiment of the invention has the following beneficial effects:
the polyurethane material wiper strip compounded and synthesized by polyether polyol, polyester polyol, alkyl hydroxyl polysiloxane and additives overcomes the defects of non-oil resistance and rapid abrasion of natural rubber materials, solves the problems of poor ultraviolet resistance, yellowing resistance, weather resistance and low-temperature resilience of common single-component polyurethane materials, and comprehensively improves the mechanical property of the wiper strip material.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be described in further detail below. In the following specific examples and comparative examples, those whose operations are not subject to the conditions mentioned above were conducted according to the conventional conditions or conditions recommended by the manufacturer.
The following examples and comparative examples illustrate the preparation of polyester polyol-1 to 6, comprising the following steps:
1) Vacuumizing the stainless steel reaction kettle, and filling nitrogen to ensure that no oxygen exists in the reaction system;
2) Phthalic anhydride, diethylene glycol, 1, 6-hexanediol, trimethylolpropane and monobutyl tin oxide as a catalyst were added in this order in the amounts of the components indicated in Table 1, with continuous introduction of nitrogen;
3) Starting stirring and raising the temperature to the temperature T 1 Keeping the temperature at t 1 In the hour, the water produced during the reaction was removed. Then the temperature is raised to the temperature T 2 Keeping the temperature at t 2 Detecting the acid value when the reaction time is short, and finishing the reaction when the acid value is lower than 3mg KOH/g; wherein, T 1 ，t 1 ，T 2 ，t 2 The values are shown in Table 2.
TABLE 1 parts by weight of polyester polyols 1 to 6
Figure BDA0003813310660000061
TABLE 2 preparation conditions of polyester polyols 1 to 6
Preparation conditions Temperature T 1 (℃) Time t 1 (h) Temperature T 2 (℃) Time t 2 (h)
Polyester polyol-1 150 1 170 10
Polyester polyol-2 145 2 175 8
Polyester polyol-3 140 3 180 6
Polyester polyol-4 150 3 175 7
Polyester polyol-5 150 2 170 8
Polyester polyol-6 140 2 180 9
The following examples and comparative examples illustrate the preparation of polyurethane prepolymers-1 to 9, comprising the steps of:
1) According to the formula given in the table 3, different polyether polyols, polyester polyols, hydroxyl polybutadiene (HTPB) and alkyl hydroxyl polysiloxane are fed and mixed according to the weight ratio, and vacuum dehydration is carried out for 2 hours under the negative pressure of 100-0.09-0.10 MPa;
2) After the water content is lower than 0.05%, cooling to 70 ℃, adding Hexamethylene Diisocyanate (HDI), heating to 85 ℃ and reacting for 3 hours;
3) And (3) cooling to 60 ℃ after the content of isocyanate groups (-NCO) reaches a theoretical final value, and carrying out vacuum defoaming for 0.5h to obtain 1-9 polyurethane prepolymers which are sealed and stored for later use.
TABLE 3 conditions of the respective Components of polyurethane prepolymers-1 to 9
Figure BDA0003813310660000062
Figure BDA0003813310660000071
The following exemplary description illustrates a method for preparing a modified nano metal oxide used in examples and comparative examples, comprising the steps of:
taking nano SiO 2 Or Al 2 O 3 Drying at 120 deg.C, cooling to room temperature, placing in a reaction kettle, adding diluted absolute ethanolDispersing and stirring the silane coupling agent solution for 0.5h by ultrasonic, taking out the solution and drying the solution in a forced air drying oven at 60 ℃ to obtain surface modified nano SiO 2 Or Al 2 O 3 。
Table 4 shows the kinds of metal oxides and the kinds of silane coupling agents used for modification in each example and comparative example:
TABLE 4 metallic oxides and silane coupling agents for modification used in examples
Figure BDA0003813310660000072
Example 1
Heating the polyurethane prepolymer-1 to 85 ℃, and adding modified nano SiO (silicon dioxide) accounting for 1.0 percent of the total amount of the system 2 Stirring 1 part of antioxidant 1010, 0.1% of silver powder, 0.3% of Tinuvin1130 and 0.1% of Tinuvin292 ultraviolet absorbent for 1 hour, adding 1, 4-butanediol serving as a chain extender (isocyanate index is adjusted and controlled to be 1.05), quickly stirring for 5 minutes, defoaming for 2 minutes in vacuum, pouring into a flat plate mold which is preheated and coated with a release agent, pressurizing and vulcanizing at 110 ℃ for 30 minutes when a gel point is reached, then demolding, and vulcanizing in an oven at 100 ℃ for 16 hours to obtain the polyurethane wiper strip material-1.
Example 2
Heating the polyurethane prepolymer-2 to 85 ℃, and adding modified nano Al accounting for 0.5 percent of the total amount of the system 2 O 3 2, 0.3 percent of antioxidant 1010, 0.5 percent of silver powder, 0.5 percent of Tinuvin1130 and 0.5 percent of Tinuvin292 ultraviolet absorbent are stirred for 1 hour, then a metered chain extender 1, 4-butanediol (isocyanate index is adjusted and controlled to be 1.03) is added, the mixture is quickly stirred for 5 minutes, the mixture is defoamed in vacuum for 2 minutes, the mixture is poured into a flat plate mould which is preheated and coated with a release agent, and when the gel point is reached, the mixture is pressurized and vulcanized for 30 minutes at 100 ℃, then is demoulded, and is vulcanized for 20 hours in a baking oven at 100 ℃, and then the polyurethane wiper strip material-2 is obtained.
Example 3
Heating the polyurethane prepolymer-3 to 85 ℃, and adding modified nano Al accounting for 2.0 percent of the total amount of the system 2 O 3 -1、0.5％The antioxidant 1010, 0.2% of silver powder, 2.0% of Tinuvin1130 and 0.3% of Tinuvin292 ultraviolet absorbent are stirred for 1 hour, then metered chain extender 1, 6-hexanediol (isocyanate index is adjusted and controlled to be 1.03) is added, the mixture is quickly stirred for 5 minutes, vacuum defoamed for 2 minutes, the mixture is poured into a flat plate mold which is preheated and coated with a release agent, when the gel point is reached, the mixture is pressurized and vulcanized for 30 minutes at 110 ℃, then the mold is released, and the mixture is vulcanized for 18 hours in a baking oven at 100 ℃, so that the polyurethane material wiper strip material-3 is obtained.
Example 4
Heating the polyurethane prepolymer-4 to 85 ℃, and adding modified nano SiO 1.5 percent of the total amount of the system 2 2, 0.4% of antioxidant 1010, 0.4% of silver powder, 1.0% of Tinuvin1130 and 0.3% of Tinuvin292 ultraviolet absorber, stirring for 1 hour, adding a metered chain extender 1, 6-hexanediol (adjusting and controlling the isocyanate index to be 1.03), quickly stirring for 5 minutes, defoaming for 2 minutes in vacuum, pouring into a flat plate mold which is preheated and coated with a release agent, pressing and vulcanizing at 110 ℃ for 30 minutes when the gel point is reached, demolding, and vulcanizing in an oven at 100 ℃ for 18 hours to obtain the polyurethane wiper strip material-4.
Example 5
Heating polyurethane prepolymer-5 to 85 ℃, adding modified nano Al accounting for 0.8 percent of the total amount of the system 2 O 3 Stirring 1, 0.3% of antioxidant 1010, 0.3% of silver powder, 2.0% of Tinuvin1130 and 0.5% of Tinuvin292 ultraviolet absorbent for 1 hour, adding metered chain extender 1, 6-hexanediol (adjusting and controlling the isocyanate index to be 1.03), quickly stirring for 5 minutes, defoaming for 2 minutes in vacuum, pouring into a flat plate mold which is preheated and coated with a release agent, pressurizing and vulcanizing at 110 ℃ for 30 minutes when the gel point is reached, demolding, and vulcanizing in a baking oven at 100 ℃ for 20 hours to obtain the polyurethane wiper strip material-5.
Example 6
Heating polyurethane prepolymer-6 to 85 ℃, adding modified nano SiO accounting for 0.5 percent of the total amount of the system 2 2, 0.3 percent of antioxidant 1010, 0.3 percent of silver powder, 2.0 percent of Tinuvin1130 and 0.5 percent of Tinuvin292 ultraviolet absorbent are stirred for 1 hour, and then metered chain extender 1, 6-hexanediol (adjusting and controlling the isocyanate index to be equal to or lower than that of the mixture)1.05 Rapidly stirring for 5min, defoaming for 2min in vacuum, pouring into a preheated flat plate mold coated with a release agent, pressurizing and vulcanizing at 110 ℃ for 30min when the gel point is reached, then demolding, and vulcanizing in an oven at 100 ℃ for 20h to obtain the polyurethane wiper strip material-6.
Comparative example 1
Heating polyurethane prepolymer-7 to 85 ℃, adding modified nano SiO accounting for 0.5 percent of the total amount of the system 2 Stirring 1, 0.3% of antioxidant 1010, 0.3% of silver powder, 2.0% of Tinuvin1130 and 0.5% of Tinuvin292 ultraviolet absorbent for 1 hour, adding metered chain extender 1, 6-hexanediol (adjusting and controlling the isocyanate index to be 1.05), quickly stirring for 5 minutes, defoaming for 2 minutes in vacuum, pouring into a flat plate mold which is preheated and coated with a release agent, pressurizing and vulcanizing at 110 ℃ for 30 minutes when the gel point is reached, demolding, and vulcanizing in a baking oven at 100 ℃ for 20 hours to obtain the polyurethane wiper strip material-7.
Comparative example 2
Heating the polyurethane prepolymer-8 to 85 ℃, and adding modified nano SiO accounting for 0.5 percent of the total amount of the system 2 Stirring 1, 0.3% of antioxidant 1010, 0.3% of silver powder, 2.0% of Tinuvin1130 and 0.5% of Tinuvin292 ultraviolet absorber for 1 hour, adding metered chain extender 1, 6-hexanediol (adjusting and controlling the isocyanate index to be 1.05), quickly stirring for 5 minutes, defoaming for 2 minutes in vacuum, pouring into a flat plate mold which is preheated and coated with a release agent, pressurizing and vulcanizing at 110 ℃ for 30 minutes when the gel point is reached, demolding, and vulcanizing in a baking oven at 100 ℃ for 20 hours to obtain the polyurethane wiper strip material-8.
Comparative example 3
Heating polyurethane prepolymer-9 to 85 ℃, adding modified nano SiO accounting for 0.5 percent of the total amount of the system 2 Stirring 1h of-1, 0.3% of antioxidant 1010, 0.3% of silver powder, 2.0% of Tinuvin1130 and 0.5% of Tinuvin292 ultraviolet absorbent, then adding a metered chain extender 1, 6-hexanediol (adjusting and controlling the isocyanate index to be 1.05), quickly stirring for 5min, defoaming for 2min in vacuum, pouring into a flat plate mould which is preheated and coated with a release agent, pressurizing and vulcanizing at 110 ℃ for 30min when the gel point is reached, then demoulding, and vulcanizing in an oven at 100 ℃ for 20h to obtain the productPolyurethane wiper strip material-9.
Comparative example 4
Heating the polyurethane prepolymer-1 to 85 ℃, and adding modified nano SiO 0.5 percent of the total amount of the system 2 Stirring 1-1 and 0.3% silver powder for 1h, adding a metered chain extender 1, 6-hexanediol (adjusting and controlling the isocyanate index to be 1.05), quickly stirring for 5min, defoaming in vacuum for 2min, pouring into a flat plate mold which is preheated and coated with a release agent, pressurizing and vulcanizing at 110 ℃ for 30min when the gel point is reached, demolding, and vulcanizing in a 100 ℃ oven for 20h to obtain the polyurethane wiper strip material-10.
The above-mentioned serial numbers of the embodiments of the present invention are only for description, and do not represent the advantages and disadvantages of the embodiments.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
The samples obtained in the above examples were aged at room temperature for one week and then tested for their properties under the following conditions:
hardness: the Shore hardness is tested according to ISO 48-1994 standard, the testing instrument is a TIME54420 Shore hardness meter produced by Peak science and technology Limited of Beijing TIMEs, the testing temperature is 25 ℃, the humidity is 46%, and the thickness of the sample is 6mm;
500% modulus and tensile strength: the preparation of the test specimens is carried out according to the regulation of GB 1039, the test standard is carried out according to ASTM D412-98a (Die D), and the test instrument is a CMT4303 type electronic universal tensile tester produced by Meitss industrial systems Limited;
wear resistance: testing according to DIN-53516 standard, wherein the minimum thickness of the sample wafer is 6mm, the testing temperature is 23 +/-2 ℃, the humidity is 40-50RH, and the testing instrument is an NBS abrasion testing machine;
the rebound resilience is as follows: testing according to BS 903 part A8;
degree of yellowing: the samples were observed for color change in appearance after exposure to sunlight for 2 months.
The data of the detailed test results of the polyurethane wiper strip materials prepared in examples 1-6 and comparative examples 1-4 are shown in table 5.
TABLE 5 Performance testing of wiper strip materials of different polyurethane materials
Figure BDA0003813310660000111
From the above data, it can be seen that if no polyester polyol or alkylhydroxypolysiloxane or hydroxyl-terminated polybutadiene or functional additive is added (comparative examples 1-4), the hardness, tensile strength, abrasion resistance and yellowing resistance of the material are somewhat diminished. The hardness of the polyurethane wiper strip materials prepared in examples 1-6 is less than or equal to the Shore H hardness A 40, the 500 percent modulus of the water scraping strip is higher than or equal to 2MPa, the tensile strength is not lower than 11MPa, and the rebound resilience higher than 69 percent in addition to the characteristics can ensure that the water scraping strip can realize better water scraping working effect in practical application; the wear rates are below 85mg/40M, and the excellent wear resistance enables the wiper strip material to achieve longer service time. The wiper strip material prepared in the embodiment is only slightly yellow after being exposed for two months, which shows that the yellowing resistance of the material is also greatly improved.
In conclusion, the technical scheme provided by the invention can realize the optimization of the polyurethane wiper strip material in the aspects of hardness, wear resistance, rebound resilience, yellowing resistance and the like, so that the polyurethane wiper strip material has excellent wiper effect and durability in practical application.

Claims (10)

1. The polyurethane wiper strip material is characterized in that the polyurethane wiper strip material comprises the following raw materials: the modified nano metal oxide-modified polyurethane comprises a polyol composition, isocyanate, a chain extender, a modified nano metal oxide and a functional additive, wherein the polyol composition comprises polyether polyol, polyester polyol, alkyl hydroxyl polysiloxane and hydroxyl-terminated polybutadiene; the chain extender is 1, 4-butanediol or 1, 6-hexanediol; the functional additive comprises an antioxidant, silver powder and an ultraviolet absorber.
2. The polyurethane wiper strip material of claim 1, wherein the polyether polyol is one or more of polyoxypropylene-polyoxyethylene glycol having a number average molecular weight of 500-3000g/mol and polytetrahydrofuran ether glycol.
3. The polyurethane wiper strip material of claim 1, wherein the polyester polyol is prepared by the steps of: vacuumizing a reaction kettle, introducing nitrogen, adding phthalic anhydride, diethylene glycol, 1, 6-hexanediol, trimethylolpropane and monobutyl tin oxide, stirring, heating to 140-150 ℃, preserving heat, removing water generated in the reaction process, heating to 170-180 ℃, preserving heat until the acid value of a reaction solution is lower than 3mgKOH/g, and finishing the reaction, wherein the phthalic anhydride: diethylene glycol: 1, 6-hexanediol: trimethylolpropane = 51-54.
4. The polyurethane wiper strip material of claim 1 wherein said alkylhydroxypolysiloxane has the following general structural formula:
Figure FDA0003813310650000011
wherein n is an integer between 5 and 20, and a + b is an integer between 4 and 10.
5. The polyurethane wiper strip material of claim 1 wherein said hydroxyl-terminated polybutadiene has a data molecular weight of 2000-4000g/mol.
6. The polyurethane wiper strip material of claim 1 wherein the isocyanate is an aliphatic diisocyanate, preferably hexamethylene diisocyanate or isophorone diisocyanate.
7. The polyurethane wiper strip material as defined in claim 1, wherein the modified nano metal oxide is added in an amount of 0.5-2.0% by weight based on the total weight of the material, and the preparation method comprises: taking nano SiO cooled to room temperature after drying 2 Or nano Al 2 O 3 Placing the mixture into a reaction kettle, adding a silane coupling agent solution diluted by absolute ethyl alcohol, performing ultrasonic dispersion, and drying to obtain surface-modified nano metal oxide; wherein the silane coupling agent is one or more of aminopropyltriethoxysilane, 3-glycidoxypropyltrimethoxysilane, gamma-aminopropylmethyldiethoxysilane, and methyltrimethoxysilane.
8. The polyurethane wiper strip material of claim 1, wherein the antioxidant is 1010, and the addition amount of the antioxidant is 0.1-0.5% of the total weight of the material; the adding amount of the silver powder is 0.2-0.5% of the total weight of the material; the ultraviolet absorbent is a composition of benzotriazole 1130 ultraviolet absorbent and hindered amine 292 light stabilizer, and the addition amounts of the ultraviolet absorbent and the hindered amine 292 light stabilizer are 0.5-2.0% and 0.1-0.5% of the total weight of the material respectively.
9. The method for preparing a wiper strip material of polyurethane material as claimed in any one of claims 1 to 8, comprising the steps of:
(A) Preparing a polyurethane prepolymer: weighing and mixing the components of the polyol composition according to a proportion, carrying out vacuum dehydration under the condition of 100-110-0.09-0.1 MPa, cooling to below 70 ℃ after the water content is lower than 0.05%, adding isocyanate, heating to 85-95 ℃ for reaction, cooling to below 60 ℃ after the isocyanate group content reaches a theoretical final value, and carrying out vacuum defoaming to obtain a polyurethane prepolymer, and carrying out closed storage for later use;
(B) Chain extension and vulcanization: heating the polyurethane prepolymer to 80-85 ℃, adding the modified nano metal oxide, the antioxidant, the silver powder and the ultraviolet absorber, uniformly stirring, adding the measured chain extender, rapidly stirring, pouring into a preheated flat plate mold coated with a release agent after vacuum defoaming, pressing and vulcanizing at 110-120 ℃ for 10-30min when the gel point is reached, demolding, and vulcanizing at 100-120 ℃ for 16-20h to obtain the polyurethane wiping strip material.
10. Use of a wiper strip material of polyurethane according to any one of claims 1 to 8 in a wiper fitting of a floor washing machine.
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DE10022276A1 (en) * 2000-05-09 2001-11-15 Basf Ag Composite material, useful for making e.g. automobile interior components, comprises a polyurethane derived from a specified polyester polyol, adhesively bonded to a thermoplastic substrate
CN102174163A (en) * 2011-01-21 2011-09-07 华南理工大学 Side chain functionalized amphiphilic polyurethane and preparation method and application thereof
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