WO2022057856A1 - 一种高***体积水性聚氨酯避孕套及其制备方法 - Google Patents

一种高***体积水性聚氨酯避孕套及其制备方法 Download PDF

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WO2022057856A1
WO2022057856A1 PCT/CN2021/118733 CN2021118733W WO2022057856A1 WO 2022057856 A1 WO2022057856 A1 WO 2022057856A1 CN 2021118733 W CN2021118733 W CN 2021118733W WO 2022057856 A1 WO2022057856 A1 WO 2022057856A1
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Prior art keywords
water
based polyurethane
drying
condom
equal
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PCT/CN2021/118733
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English (en)
French (fr)
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戴家兵
冯林林
刘斌
陈亮
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兰州科时西西里健康科技有限公司
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Priority to JP2023518123A priority Critical patent/JP2023541693A/ja
Priority to EP21868678.0A priority patent/EP4215570A1/en
Priority to CA3196032A priority patent/CA3196032A1/en
Priority to US18/245,764 priority patent/US20230390104A1/en
Priority to MX2023003223A priority patent/MX2023003223A/es
Priority to AU2021345853A priority patent/AU2021345853A1/en
Publication of WO2022057856A1 publication Critical patent/WO2022057856A1/zh

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    • B29C41/00—Shaping by coating a mould, core or other substrate, i.e. by depositing material and stripping-off the shaped article; Apparatus therefor
    • B29C41/02—Shaping by coating a mould, core or other substrate, i.e. by depositing material and stripping-off the shaped article; Apparatus therefor for making articles of definite length, i.e. discrete articles
    • B29C41/14—Dipping a core
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B29C41/00—Shaping by coating a mould, core or other substrate, i.e. by depositing material and stripping-off the shaped article; Apparatus therefor
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    • C08G18/4808—Mixtures of two or more polyetherdiols
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
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    • C08G18/4804—Two or more polyethers of different physical or chemical nature
    • C08G18/4812—Mixtures of polyetherdiols with polyetherpolyols having at least three hydroxy groups
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    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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    • C08G18/4825—Polyethers containing two hydroxy groups
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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    • C—CHEMISTRY; METALLURGY
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    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
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    • C08J2375/04—Polyurethanes
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Definitions

  • the invention relates to the technical application field of water-based polyurethane, in particular to a high-explosive-volume water-based polyurethane condom and a preparation method thereof.
  • Condoms are the most widely used and simple devices for contraception and prevention of sexually transmitted diseases in the world.
  • the existing products mainly include natural latex rubber condoms and water-based polyurethane condoms.
  • natural latex rubber condoms Due to the material properties of natural latex, the thickness of natural latex rubber condoms is difficult to be less than 0.04mm. At the same time, natural latex contains a variety of proteins, and there are certain safety risks for people with protein allergies. However, after decades of marketization, natural latex rubber condoms have a wide market audience, and their soft texture has been recognized by consumers.
  • polyurethane condoms on the market generally have high modulus, and the burst volume is about 7-11 liters. Compared with latex, its softness and burst volume are poor. Therefore, a water-based polyurethane with low modulus and high elongation was developed. Condoms not only retain the advantages of polyurethane without protein allergy, high strength, high pressure, and high thermal conductivity, but also have the softness and high blasting volume close to latex products, which further enhances the experience of polyurethane condom products. It is very important market significance.
  • the present invention provides a high-bursting volume aqueous polyurethane condom and a preparation method thereof.
  • the present invention first provides a high-bursting volume water-based polyurethane condom and a preparation method thereof.
  • drying after crimping the water-based polyurethane film is molding drying
  • drying after dipping the water-based polyurethane is molding drying
  • t is the molding drying time
  • t is the shaping drying time
  • N is the number of dipping repetitions
  • ⁇ 2.7-0.015 ⁇ T
  • T is the temperature of shaping drying and forming drying
  • the unit of T is degrees Celsius
  • the unit of t and t is minutes.
  • the shaping drying time is 2-10 minutes
  • the molding drying time is 10-65 minutes
  • the isolating agent drying time is 2-30 minutes.
  • the drying temperature is 80-140°C.
  • the solid content of the waterborne polyurethane is 15-30%.
  • the macromolecular polyol in the solid raw material component of the water-based polyurethane accounts for 60-85% of all the solid raw material components, and in the macromolecular polyol, there are three or more functionalities.
  • the proportion of macromolecular polyols is 10-40%.
  • the macromolecule polyol is composed of a difunctional macromolecule polyol with a molecular mass of 500-4000 and a trifunctional macromolecule polyol with a molecular mass of 650-6000 according to a mass ratio of 4: (0.2- 1.5) Composition.
  • the present invention also provides an aqueous polyurethane condom prepared by the above method.
  • the thickness of the water-based polyurethane condom is 0.02mm-0.06mm.
  • the water-based polyurethane condom includes any one or more of the following features:
  • 100% tensile modulus is less than or equal to 2.0MPa
  • the blasting volume is greater than or equal to 12 liters
  • the burst pressure is greater than or equal to 1KPa;
  • the elongation at break is greater than or equal to 650%
  • the tensile strength is greater than or equal to 20MPa.
  • the present invention provides a low-modulus and high-explosive-volume polyurethane condom and a preparation method thereof, which have the following beneficial effects: the present invention adopts a low-modulus and high-elongation water-based polyurethane resin, which is dipped and baked for many times.
  • the dry molding process enables the prepared polyurethane condoms with low modulus and high blasting volume to achieve product thickness of 0.02-0.06mm, 100% tensile modulus ⁇ 2.0MPa, blasting volume ⁇ 12 liters, and blasting pressure ⁇ 1KPa. .
  • Figure 1 shows a schematic flow diagram of the preparation method of the present invention.
  • the present invention first provides a kind of preparation method of high-bursting volume water-based polyurethane condom, described method can comprise adopting the mode of repeatedly impregnating water-based polyurethane resin to realize, and described method comprises the steps of S1-S4 at least:
  • the water-based polyurethane is an anionic water-based polyurethane
  • the 100% tensile modulus of the water-based polyurethane is less than or equal to 2.0MPa
  • the elongation at break is greater than or equal to 650%.
  • step S1 in order to prepare the water-based polyurethane condom, the present invention provides an anionic water-based polyurethane with good tensile modulus and elongation at break, and the 100% tensile modulus of the anionic polyurethane can be less than or equal to 2.0MPa, such as 1.8MPa, 1.5MPa, 1.4MPa, 1.3MPa, the elongation at break of the anionic water-based polyurethane can be greater than or equal to 650%, such as 720%, 730%, 750%, the water-based polyurethane provided by the present invention can make the final
  • the prepared water-based polyurethane condom has the excellent performance that the burst volume is greater than 12 liters.
  • the anionic water-based polyurethane resin used in the present invention has a mature technology and has the advantage of large molecular weight under the premise of low modulus.
  • the solid content of the water-based polyurethane resin It can be between 15-30%, such as 20%, 25%, the water-based polyurethane resin has better resin leveling in the above solid content range, the uniformity difference of the prepared condom is small, the blasting volume is large, and the defect is small.
  • the water-based polyurethane of the present invention can be synthesized by a step-by-step method.
  • the water-based polyurethane can be prepared from solid raw materials and dispersed in water.
  • the step-by-step method can include processes such as polymerization, chain extension, and emulsification.
  • the solid raw material may include a soft segment and a hard segment
  • the soft segment may be a macromolecule polyol or a combination of macromolecule polyols
  • the hard segment may be a polyisocyanate or a composition of polyisocyanates
  • the macromolecule polyol Molecular polyols may include macromolecular diols and macromolecular triols, such as polytetrahydrofuran glycol (PTMEG), polypropylene glycol (PPG), and propylene oxide triols.
  • the molecular weight of the polytetrahydrofuran diol may be 500-4000
  • the molecular weight of the polypropylene glycol may be 1000-5000
  • the molecular weight of the propylene oxide triol may be 650-6000.
  • the water-based polyurethane is composed of the following solid raw materials and parts by weight: 23-38 parts of macromolecular diols, 3-5 parts of macromolecular triols, 6.5-10 parts of polyisocyanates, 1.3-1.6 parts of hydrophilic chain extender, 0.05-0.08 parts of small molecular polyol chain extender, 1-1.3 parts of neutralizer, 0.2-0.3 parts of small molecular amine post-chain extender, 0.05-0.08 parts of catalyst.
  • the hydrophilic chain extender can be one or more of dimethylol propionic acid, dimethylol butyric acid, and sodium ethylenediamine ethanesulfonate
  • the small molecule polyol chain extender can include trihydroxy Any one or more of methyl propane, glycerol, butanediol, ethylene glycol and cyclohexanedimethanol
  • the neutralizing agent can include any one or more of triethylamine and sodium bicarbonate
  • the small molecular amine post-chain extender is any one or more of ethylenediamine, hexamethylenediamine, isophoronediamine, toluenediamine and diaminodicyclohexylmethane.
  • the polyisocyanate can be any one or more of TDI, MDI, IPDI, HDI, and HMDI.
  • the water-based polyurethane is composed of the following solid raw materials and parts by weight: 8-13 parts of PTMEG, 15-25 parts of PPG, 3-5 parts of propylene oxide triol, 5.5-8 parts of IPDI, 1-2 parts HDI, 1.3-1.6 parts DMPA and 0.5-0.8 parts DEG, 0.05-0.08 parts catalyst, 1-1.3 parts triethylamine, 0.2-0.3 parts isophoronediamine .
  • the macromolecule polyol is composed of a difunctional macromolecule polyol with a molecular mass of 500-4000 and a trifunctional macromolecule polyol with a molecular mass of 650-6000 according to a mass ratio of 4: (0.2- 1.5) Composition, further, the macromolecular polyol is composed of polytetrahydrofuran diol (PTMEG) with a molecular mass of 500-4000, polypropylene glycol (PPG) with a molecular mass of 1000-5000 and an oxidized polyol with a molecular mass of 650-6000.
  • PTMEG polytetrahydrofuran diol
  • PPG polypropylene glycol
  • the propylene triol is composed according to the mass ratio of 1:3:(0.2-1.5).
  • the proportion of soft segment in the water-based polyurethane resin can account for 60-85% of all solid raw materials, such as 79.5%, and the cross-linking ratio of the soft segment can be 10-40%, such as 25%.
  • the definition can be: the mass ratio of macromolecular polyols with three or more functionalities to the whole macromolecular polyols.
  • the preparation of the water-based polyurethane condom also includes a process of dipping and drying multiple times to form a water-based polyurethane film.
  • the mold can be dipped in the water-based polyurethane and then dried, and repeated N times to Realization, wherein the number of repetitions N can be 1-5 times, such as 2 times, 3 times, the present invention can make the thickness uniformity of the condom good, less defects, and large blasting volume through the multiple dipping process, which is conducive to drying without wrinkling and cracking.
  • the water-based polyurethane of the present invention needs to undergo a drying step after each dipping, and the drying after each dipping may be shaping drying, and the shaping drying time may be 2-10 minutes.
  • step S3 the water-based polyurethane adhesive film may be dried again after being curled, and the drying may be molding drying, and the molding drying time may be 10-65 minutes.
  • the drying temperature may be 80-140°C, such as 120°C and 130°C.
  • the tensile strength of the polyurethane after being dipped and dried into a film can be tested after each dipping of the polyurethane. For example, when the tensile strength of the polyurethane dipped and dried into a film can reach 60% of the predetermined tensile strength The drying can be stopped and the next dipping can be performed.
  • the predetermined tensile strength can be, for example, greater than or equal to 20 MPa. According to the present invention, drying is performed for a certain period of time after each dipping, such as the stretching of the polyurethane film after the first dipping. The strength is tested.
  • the drying time used at this time can be the shaping drying time described in the present invention.
  • the shaping drying time used in the present invention The drying time may be greater than or equal to the drying time taken for the tensile strength of the polyurethane film formed by the first immersion in the water-based polyurethane to reach 60% of the predetermined tensile strength.
  • the forming drying temperature is the same as the shaping drying temperature.
  • the above-mentioned relationship between the shaping drying time and the forming drying time can make the final prepared condoms have the best performance, and avoid the final prepared products being too brittle due to too long drying time or too short time. Defects of insufficient strength.
  • step S4 the drying time after dipping the release agent may be 2-30 minutes.
  • the present invention also provides a water-based polyurethane condom with low modulus and high burst volume.
  • the water-based polyurethane condom can be a thin condom, and its thickness can be between 0.02mm-0.06mm, such as 0.03mm,
  • the polyurethane condom has good tensile modulus and burst volume, and the 100% tensile modulus of the polyurethane condom of the present invention can be less than or equal to 2.0 MPa, such as 1.8 MPa, 1.3 MPa, 1.4 MPa, and the polyurethane contraceptive
  • the burst volume of the condom can be greater than 12 liters, such as 15 liters, 17 liters, 18 liters, 20 liters, and in one embodiment, the polyurethane condom also has a good elongation at break, and the elongation at break of the polyurethane condom Can be greater than or equal to 650%, such as 720%, 750%, the burst pressure of
  • the PTMEG 3000 of 4.73kg and the PPG3000 of 9.47kg, the 5000 molecular weight oxypropylene triol of 4.2kg are dropped into the reactor, the IPDI of 2.92kg and the HDI of 0.75kg are dropped, stirring is warming up to 80-120 °C, insulation reaction 1-3 hour, add the DMPA of 0.72kg, the DEG of 0.31kg, the acetone of 6.5kg and the catalyzer of 0.04kg, react at 70-90 °C for 2-6 hours, then add water to lower the temperature and add triethylamine to neutralize and carry out high-speed dispersion emulsification, Then, 0.15 kg of isophorone diamine was added to carry out post-chain extension, and then vacuum precipitation was carried out to obtain the desired aqueous polyurethane resin emulsion.
  • the 100% tensile modulus of the prepared polyurethane resin was 1.69 MPa, and the elongation at break was 811%.
  • sample 1 The glass mold was cleaned, the surface of the mold was heated to 30-40°C, and the polyurethane resin prepared above was dipped for 5 times. Molding and drying for 10.8 minutes, then immersed in release agent, dried at 80°C, demolded, and subjected to electrical inspection, internal packaging, and outsourcing to obtain sample 1.
  • the thickness of sample 1 is 0.032mm, and the 100% tensile modulus of sample 1 is 100%. It is 1.7MPa, the burst volume is 18.9 liters, the elongation at break is 805%, the burst pressure is 2.8KPa, and the tensile strength is 33MPa.
  • Example 2 The glass mold was cleaned, the surface of the mold was heated to 30-40°C, and the polyurethane resin obtained in Example 1 was dipped for 4 times. Forming and drying were carried out for 27 minutes, then immersed in release agent, and dried at 80°C. After demolding, electrical inspection, internal packaging, and external packaging were carried out to obtain sample 2. The thickness of sample 2 was 0.038mm, and the 100% stretch of sample 2 was carried out.
  • the modulus is 1.69MPa
  • the burst volume is 19.5 liters
  • the elongation at break is 812%
  • the burst pressure is 3.7KPa
  • the tensile strength is 32MPa.
  • Example 2 The glass mold was cleaned, the surface of the mold was heated to 30-40°C, and the polyurethane resin obtained in Example 1 was dipped three times. Forming and drying were carried out for 63 minutes, then immersed in release agent, and dried at 80°C. After demolding, electrical inspection, internal packaging, and external packaging were carried out to obtain sample 3.
  • the thickness of sample 3 was 0.026 mm, and the 100% tensile strength of sample 3 was obtained.
  • the modulus was 1.67 MPa
  • the burst volume was 18.2 liters
  • the elongation at break was 801%
  • the burst pressure was 2.0 KPa
  • the tensile strength 30 MPa.
  • Comparative Example 1 and Example 2 The preparation conditions of Comparative Example 1 and Example 2 are the same, and the molding drying time of Sample 2 in Example 2 is changed to 37 minutes to obtain Comparative Sample 1.
  • the product thickness of Comparative Sample 1 is 0.038mm, and the 100% stretching die
  • the volume is 1.9MPa
  • the burst volume is 15.4 liters
  • the elongation at break is 721%
  • the burst pressure is 2.KPa
  • the tensile strength is 25MPa.
  • Comparative Example 2 The preparation conditions of Comparative Example 2 and Example 2 are the same, and the molding drying time of Sample 2 in Example 2 is changed to 32 minutes to obtain Comparative Sample 2.
  • the product thickness of Comparative Sample 2 is 0.038mm and 100% tensile modulus. It is 1.79MPa, the burst volume is 16.2 liters, the elongation at break is 761%, the burst pressure is 2.4KPa, and the tensile strength is 26.5MPa.
  • Comparative Example 3 and Example 2 The preparation conditions of Comparative Example 3 and Example 2 are the same, and the molding drying time of Sample 2 in Example 2 is changed to 22 minutes to obtain Comparative Sample 3.
  • the product thickness of Comparative Sample 3 is 0.038mm, and the 100% stretching die
  • the volume is 1.54MPa
  • the burst volume is 21.2 liters
  • the elongation at break is 856%
  • the burst pressure is 2.6KPa
  • the tensile strength is 27.3MPa.
  • Comparative Example 4 and Example 2 The preparation conditions of Comparative Example 4 and Example 2 are the same, and the molding drying time of Sample 2 in Example 2 is changed to 17 minutes to obtain Comparative Sample 4.
  • the product thickness of Comparative Sample 4 is 0.038mm, and the 100% stretching die
  • the volume is 1.3MPa, the burst volume is 24 liters, the elongation at break is 921%, the burst pressure is 1.6KPa, and the tensile strength is 23.1MPa.
  • the present invention effectively overcomes various shortcomings in the prior art and has high industrial utilization value.
  • the above-mentioned embodiments merely illustrate the principles and effects of the present invention, but are not intended to limit the present invention.
  • anyone skilled in the art can modify or change the above embodiments without departing from the spirit and scope of the present invention. Therefore, all equivalent modifications or changes made by those with ordinary knowledge in the technical field without departing from the spirit and technical idea disclosed in the present invention should still be covered by the claims of the present invention.

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Abstract

本发明提供了一种高***体积水性聚氨酯避孕套及其制备方法，所述方法包括以下步骤：提供一水性聚氨酯；浸渍所述水性聚氨酯后烘干，并重复N次浸渍水性聚氨酯后烘干工序以得到一水性聚氨酯胶膜；卷边所述水性聚氨酯胶膜后烘干；浸渍隔离剂再经烘干、脱模、电检得到所述水性聚氨酯避孕套；其中，N＝1-5，所述水性聚氨酯为阴离子型水性聚氨酯，所述水性聚氨酯的100％拉伸模量小于等于2.0MPa，断裂延伸率大于等于650％，经过所述方法制备得到的聚氨酯避孕套***体积大于12升，***压力大于1KPa，100％拉伸模量小于等于2.0MPa。

Description

一种高***体积水性聚氨酯避孕套及其制备方法 技术领域
本发明涉及水性聚氨酯技术应用领域，具体的涉及一种高***体积水性聚氨酯避孕套及其制备方法。
背景技术
避孕套是目前世界上应用最为广泛和简单的避孕以及防止性病传播的器具，现有产品主要有天然胶乳橡胶避孕套和水性聚氨酯避孕套。
天然胶乳橡胶避孕套由于天然胶乳的材料特性，厚度难以做到0.04mm以下，同时天然胶乳中含有多种蛋白质，蛋白过敏人群使用会存在一定的安全风险。但天然胶乳橡胶避孕套经过几十年的市场化，其市场受众广泛，同时其质地柔软得到了消费者的认可。
目前市面上的聚氨酯避孕套普遍模量较高，***体积为7-11升左右，相对于乳胶来说，其柔软性和***体积较差，因此开发出一款低模量高延伸的水性聚氨酯避孕套，既保留聚氨酯的无蛋白过敏，高强度、高压力、高导热性的优点，同时拥有接近乳胶产品的柔软性和高***体积，进一步提升聚氨酯避孕套产品的体验感，有十分重要的市场意义。
发明内容
为解决上述现有技术中存在的问题，本发明提供一种高***体积水性聚氨酯避孕套及其制备方法。
本发明首先提供了一种高***体积水性聚氨酯避孕套及其制备方法，所述方法至少包括以下步骤：提供一水性聚氨酯；浸渍所述水性聚氨酯后烘干，并重复N次浸渍所述水性聚氨酯后烘干工序以得到一水性聚氨酯胶膜；卷边所述水性聚氨酯胶膜后烘干；浸渍隔离剂再经烘干、脱模、电检得到所述水性聚氨酯避孕套；其中，N＝1-5，所述水性聚氨酯为阴离子型水性聚氨酯，所述水性聚氨酯的100％拉伸模量小于等于2.0MPa，断裂延伸率大于等于650％。
在一实施例中，卷边所述水性聚氨酯胶膜后烘干为成型烘干，浸渍所述水性聚氨酯后烘干为定型烘干，所述定型烘干时间和所述成型烘干时间具有t 成＝90·Φ-1.8·(N+2)t 定的关系，其中t 成为成型烘干时间，t 定为定型烘干时间，N为浸渍重复的次数，Φ＝2.7-0.015·T，T为定型烘干以及成型烘干的温度，T的单位为摄氏度，t 定以及t 成的单位为分钟。
在一实施例中，所述定型烘干时间为2-10分钟，所述成型烘干时间为10-65分钟，所述隔离剂烘干时间为2-30分钟。
在一实施例中，所述烘干温度为80-140℃。
在一实施例中，所述水性聚氨酯的固含量为15-30％。
在一实施例中，所述水性聚氨酯的固体原料组分中大分子多元醇占所有固体原料组分的60-85％，在所述大分子多元醇中，具有三个及三个以上官能度的大分子多元醇的占比为10-40％。
在一实施例中，所述大分子多元醇由分子质量为500-4000的二官能度大分子多元醇以及分子质量为650-6000的三官能度大分子多元醇按照质量比4：(0.2-1.5)组成。
本发明还提供了一种如上所述方法制备得到的水性聚氨酯避孕套。
在一实施例中，所述水性聚氨酯避孕套的厚度为0.02mm-0.06mm。
在一实施例中，所述水性聚氨酯避孕套包括以下特征中的任意一项或多项：
100％拉伸模量小于等于2.0MPa；
***体积大于等于12升；
***压力大于等于1KPa；
断裂延伸率大于等于650％；
拉伸强度大于等于20MPa。
如上所述，本发明提供了一种低模量高***体积的聚氨酯避孕套及其制备方法，具有以下有益效果：本发明通过采用低模量高延伸率的水性聚氨酯树脂，通过多次浸渍烘干成型工艺，使得制备得到的低模量高***体积的聚氨酯避孕套可以达到产品厚度0.02-0.06mm、100％拉伸模量≤2.0MPa、***体积≥12升、***压力≥1KPa的性能指标。
附图说明
图1显示为本发明制备方法的流程示意图。
具体实施方式
以下通过特定的具体实例说明本发明的实施方式，本领域技术人员可由本说明书所揭露的内容轻易地了解本发明的其他优点与功效。本发明还可以通过另外不同的具体实施方式加以实施或应用，本说明书中的各项细节也可以基于不同观点与应用，在没有背离本发明的精神下进行各种修饰或改变。注意，本发明所述聚氨酯树脂以及所述避孕套的性能测试分别参照国家标准GB/T1040.1-2006、GB7544-2009进行。如没有特别说明，本文中所示的“％”和“份”分别是指“质量％”和“质量份”。
请参阅图1。本发明首先提供了一种高***体积水性聚氨酯避孕套的制备方法，所述方 法可以包括采用多次浸渍水性聚氨酯树脂的方式来实现，所述方法至少包括S1-S4的步骤：
S1：提供一水性聚氨酯；
S2：浸渍所述水性聚氨酯后烘干，并重复N次浸渍水性聚氨酯后烘干工序以得到一水性
聚氨酯胶膜；
S3：卷边所述水性聚氨酯胶膜后烘干；
S4：浸渍隔离剂再经烘干、脱模、电检得到所述水性聚氨酯避孕套；
其中，N＝1-5，所述水性聚氨酯为阴离子型水性聚氨酯，所述水性聚氨酯的100％拉伸模量小于等于2.0MPa，断裂延伸率大于等于650％。
在步骤S1中，本发明为了制备所述水性聚氨酯避孕套，提供了一种具有良好拉伸模量以及断裂伸长率的阴离子水性聚氨酯，所述阴离子聚氨酯的100％拉伸模量可以小于等于2.0MPa，例如1.8MPa、1.5MPa、1.4MPa、1.3MPa，所述阴离子水性聚氨酯的断裂延伸率可以大于等于650％，例如720％，730％，750％，本发明提供的水性聚氨酯可以使得最终制备得到的水性聚氨酯避孕套具有***体积大于12升的优异性能，本发明采用的阴离子水性聚氨酯树脂工艺成熟，具有在低模量的前提下分子量较大的优势，所述水性聚氨酯树脂的固含量可以是在15-30％之间，例如20％，25％，所述水性聚氨酯树脂在以上固含量区间具有树脂流平较好，制备得到的避孕套均匀度差异小，***体积大，缺陷少的优势。
本发明所述水性聚氨酯可以采用分步法合成，所述水性聚氨酯可以由固份原料制备并分散在水中形成，所述分步法可以包括有聚合、扩链、乳化等过程，所述水性聚氨酯固份原料中可以包括有软段和硬段，所述软段可以是大分子多元醇或者大分子多元醇的组合物，所述硬段可以是多异氰酸酯或者多异氰酸酯的组合物，所述大分子多元醇可以包括有大分子二元醇和大分子三元醇，例如可以是聚四氢呋喃二醇(PTMEG)、聚丙二醇(PPG)、氧化丙烯三元醇中的多种。其中，所述聚四氢呋喃二醇的分子量可以是500-4000，所述聚丙二醇的分子量可以是1000-5000，所述氧化丙烯三元醇的分子量可以是650-6000。
在一实施例中，所述水性聚氨酯由以下固份原料及重量份组成：23-38份的大分子二元醇，3-5份的大分子三元醇，6.5-10份的多异氰酸酯，1.3-1.6份的亲水扩链剂，0.05-0.08的小分子多元醇扩链剂，1-1.3份的中和剂，0.2-0.3份的小分子胺后扩链剂，0.05-0.08份的催化剂。
所述亲水扩链剂可以是二羟甲基丙酸、二羟甲基丁酸、乙二胺基乙磺酸钠一种或多种，所述小分子多元醇扩链剂可以包括三羟甲基丙烷、甘油、丁二醇、乙二醇和环己二甲醇中的任意一种或多种，所述中和剂可以包括三乙胺、碳酸氢钠中的任意一种或多种，所述小分子胺后扩链剂为乙二胺、己二胺、异氟尔酮二胺、甲苯二胺和二氨基二环己基甲烷中的任意一 种或多种。所述多异氰酸酯可以是中的TDI，MDI，IPDI，HDI，HMDI中的任意一种或多种。
在一实施例中，所述水性聚氨酯由以下固份原料及重量份组成：8-13份的PTMEG，15-25份的PPG，3-5份的氧化丙烯三元醇，5.5-8份的IPDI，1-2份的HDI，1.3-1.6份的DMPA和0.5-0.8份的DEG，0.05-0.08份的催化剂，1-1.3份的三乙胺，0.2-0.3份的异佛尔酮二胺。
在一实施例中，所述大分子多元醇由分子质量为500-4000的二官能度大分子多元醇以及分子质量为650-6000的三官能度大分子多元醇按照质量比4：(0.2-1.5)组成，进一步的，所述大分子多元醇由分子质量为500-4000的聚四氢呋喃二醇(PTMEG)、分子质量为1000-5000的聚丙二醇(PPG)以及分子质量为650-6000的氧化丙烯三元醇按照质量比1：3：(0.2-1.5)组成。
所述水性聚氨酯树脂中软段比例可以占所有固份原料的60-85％，例如79.5％，所述软段交联比可以是10-40％，例如25％，所述软段交联比的定义可以是：有三个以及三个以上官能度的大分子多元醇占整个大分子多元醇的质量比值。
在步骤S2中，所述水性聚氨酯避孕套的制备还包括有多次浸渍并烘干以形成一水性聚氨酯胶膜的过程，例如可以将模具浸渍所述水性聚氨酯后烘干，并重复N次来实现，其中重复次数N可以是1-5次，例如2次、3次，本发明通过多次浸渍工艺可以使得避孕套厚度均匀度好，缺陷少，***体积大，利于烘干不皱不开裂。本发明所述水性聚氨酯每次浸渍后都需要经过烘干的步骤，所述每次浸渍后的烘干可以为定型烘干，所述定型烘干时间可以是2-10分钟。
在步骤S3中，所述水性聚氨酯胶膜经过卷边后还可以进行再次烘干，所述烘干可以是成型烘干，所述成型烘干时间可以是10-65分钟。在步骤S2-S4中，所述烘干温度可以是80-140℃，例如120℃、130℃。
本发明每次浸渍聚氨酯后可以对所述聚氨酯浸渍烘干成膜后的拉伸强度进行测试，例如，每次聚氨酯浸渍烘干成膜后的拉伸强度可以达到预定拉伸强度的60％时就可以停止烘干并进行下一次浸渍，所述预定拉伸强度例如可以是大于等于20MPa，本发明所述每次浸渍后烘干一定时间，例如第一次浸渍后对聚氨酯成膜的拉伸强度进行测试，如果聚氨酯成膜后的拉伸强度可以达到预定拉伸强度的60％时，此时采用的烘干时间就可以是本发明所述的定型烘干时间，本发明采用的定型烘干时间可以大于等于第一次浸渍水性聚氨酯形成的聚氨酯膜拉伸强度达到预定拉伸强度60％所用的烘干时间。所述成型烘干时间可以遵循t 成＝90·Φ-1.8·(N+2)t 定的关系，其中t 成为成型烘干时间，t 定为定型烘干时间，N为浸渍重复的次数，Φ为温度影响因子，Φ＝2.7-0.015·T，T为定型烘干以及成型烘干的温度，T的单位为摄氏度，所述成型 烘干时间以及定型烘干时间的单位为分钟，在一实施例中，利用上述关系式时，所述成型烘干温度和所述定型烘干温度相同。所述定型烘干时间和成型烘干时间采用上述关系可以使得最后制备得到的避孕套性能最佳，避免最后制备得到的产品因为烘干时间过长带来的过脆或者时间太短带来的强度不够的缺陷。
在步骤S4中，所述浸渍隔离剂后的烘干时间可以是2-30分钟。
本发明还提供了一种低模量高***体积的水性聚氨酯避孕套，所述水性聚氨酯避孕套可以是一种薄款避孕套，其厚度可以在0.02mm-0.06mm之间，例如0.03mm，所述聚氨酯避孕套具有良好的拉伸模量以及***体积，本发明所述聚氨酯避孕套的100％拉伸模量可以小于等于2.0MPa，例如1.8MPa、1.3MPa、1.4MPa，所述聚氨酯避孕套的***体积可以大于12升，例如15升、17升、18升、20升，在一实施例中，所述聚氨酯避孕套还具有良好的断裂延伸率，所述聚氨酯避孕套的断裂延伸率可以是大于等于650％，例如720％，750％，所述避孕套***压力可以大于等于1KPa，例如1.3KPa、1.4KPa，所述聚氨酯避孕套的拉伸强度可以大于等于20MPa，例如30MPa、31MPa、32MPa、33MPa。此处，所述聚氨酯避孕套可以为男用避孕套，应当理解，其还可以制成为女用避孕套，以及其他的异型避孕套等。
以下将引入具体的实施例对本发明进行更为详细的说明。
实例
实施例1
将4.73kg的PTMEG 3000和9.47kg的PPG3000，4.2kg的5000分子量氧化丙烯三元醇投入反应釜，投入2.92kg的IPDI和0.75kg的HDI，搅拌升温至80-120℃，保温反应1-3小时，加入0.72kg的DMPA、0.31kg的DEG、6.5kg的丙酮及0.04kg的催化剂，在70-90℃下反应2-6小时，然后降温加入三乙胺中和后加水进行高速分散乳化，然后加入0.15kg的异佛尔酮二胺进行后扩链，再进行真空脱溶，得到所需的水性聚氨酯树脂乳液。经过测量制备得到的聚氨酯树脂的100％拉伸模量为1.69MPa，断裂延伸率为811％。
将玻璃模具清洗干净，模具表面加热到30-40℃，浸渍上述制备得到的聚氨酯树脂5次，每次浸渍后在140℃条件下进行定型烘干4分钟，卷边后在140℃条件下进行成型烘干10.8分钟，然后浸渍隔离剂，在80℃条件下烘干，脱模后进行电检、内包、外包，得到样品1，样品1厚度为0.032mm，样品1的100％拉伸模量为1.7MPa，***体积为18.9升，断裂延伸率为805％，***压力为2.8KPa，拉伸强度为33MPa。
实施例2
将玻璃模具清洗干净，模具表面加热到30-40℃，浸渍实施例1得到的聚氨酯树脂4次，每次浸渍后在120℃条件下进行定型烘干6分钟，卷边后在120℃条件下进行成型烘干27分钟，然后浸渍隔离剂，在80℃条件下烘干，脱模后进行电检、内包、外包，得到样品2，样品2的厚度为0.038mm，样品2的100％拉伸模量为1.69MPa，其***体积19.5升，断裂延伸率为812％，***压力为3.7KPa，拉伸强度为32MPa。
实施例3
将玻璃模具清洗干净，模具表面加热到30-40℃，浸渍实施例1得到的聚氨酯树脂3次，每次浸渍后在80℃条件下进行定型烘干10分钟，卷边后在80℃条件下进行成型烘干63分钟，然后浸渍隔离剂，在80℃条件下烘干，脱模后进行电检、内包、外包，得到样品3，样品3的厚度为0.026mm，样品3的100％拉伸模量为1.67MPa，***体积为18.2升，断裂延伸率为801％，***压力为2.0KPa，拉伸强度为30MPa。
对比例1
对比例1和实施例2的制备条件相同，将实施例2中的样品2的成型烘干时间变为37分钟，得对比样1，对比样1的产品厚度为0.038mm，100％拉伸模量为1.9MPa，***体积15.4升，断裂延伸率为721％，***压力为2.KPa，拉伸强度为25MPa。
对比例2
对比例2和实施例2的制备条件相同，将实施例2中的样品2的成型烘干时间变为32分钟，得到对比样2，对比样2的产品厚度0.038mm，100％拉伸模量为1.79MPa，***体积为16.2升，断裂延伸率761％，***压力为2.4KPa，拉伸强度为26.5MPa。
对比例3
对比例3和实施例2的制备条件相同，将实施例2中的样品2的成型烘干时间变为22分钟，得到对比样3，对比样3的产品厚度为0.038mm，100％拉伸模量1.54MPa，其***体积21.2升，断裂延伸率856％，***压力2.6KPa，拉伸强度27.3MPa。
对比例4
对比例4和实施例2的制备条件相同，将实施例2中的样品2的成型烘干时间变为17分钟，得到对比样4，对比样4的产品厚度为0.038mm，100％拉伸模量为1.3MPa，***体积为24升，断裂延伸率为921％，***压力为1.6KPa，拉伸强度为23.1MPa。
所以，本发明有效克服了现有技术中的种种缺点而具高度产业利用价值。上述实施例仅例示性说明本发明的原理及其功效，而非用于限制本发明。任何熟悉此技术的人士皆可在不违背本发明的精神及范畴下，对上述实施例进行修饰或改变。因此，举凡所属技术领域中具有通常知识者在未脱离本发明所揭示的精神与技术思想下所完成的一切等效修饰或改变，仍应由本发明的权利要求所涵盖。

Claims (10)

  1. 一种高***体积水性聚氨酯避孕套的制备方法，其特征在于，所述方法至少包括以下步骤：
    提供一水性聚氨酯；
    浸渍所述水性聚氨酯后烘干，并重复N次浸渍所述水性聚氨酯后烘干工序以得到一水性聚氨酯胶膜；
    卷边所述水性聚氨酯胶膜后烘干；
    浸渍隔离剂再经烘干、脱模、电检得到所述水性聚氨酯避孕套；
    其中，N＝1-5，所述水性聚氨酯为阴离子型水性聚氨酯，所述水性聚氨酯的100％拉伸模量小于等于2.0MPa，断裂延伸率大于等于650％。
  2. 根据权利要求1所述的方法，其特征在于：卷边所述水性聚氨酯胶膜后烘干为成型烘干，
    浸渍所述水性聚氨酯后烘干为定型烘干，所述定型烘干时间和所述成型烘干时间具有t 成＝90·Φ-1.8·(N+2)·t 定的关系，其中t 成为成型烘干时间，t 定为定型烘干时间，N为浸渍重复的次数，Φ＝2.7-0.015·T，T为定型烘干以及成型烘干的温度，T的单位为摄氏度，t 定以及t 成的单位为分钟。
  3. 根据权利要求2所述的方法，其特征在于：所述定型烘干时间为2-10分钟，所述成型烘干时间为10-65分钟，所述隔离剂烘干时间为2-30分钟。
  4. 根据权利要求2所述的方法，其特征在于：所述烘干温度为80-140℃。
  5. 根据权利要求1所述的方法，其特征在于：所述水性聚氨酯的固含量为15-30％。
  6. 根据权利要求1所述的方法，其特征在于：所述水性聚氨酯的固体原料组分中大分子多元醇占所有固体原料组分的60-85％，在所述大分子多元醇中，具有三个及三个以上官能度的大分子多元醇的占比为10-40％。
  7. 根据权利要求6所述的方法，其特征在于：所述大分子多元醇由分子质量为500-4000的二官能度大分子多元醇以及分子质量为650-6000的三官能度大分子多元醇按照质量比4：(0.2-1.5)组成。
  8. 一种根据权利要求1-7任意所述方法制备得到的高***体积水性聚氨酯避孕套。
  9. 根据权利要求8所述的水性聚氨酯避孕套，其特征在于：所述水性聚氨酯避孕套的厚度为0.02mm-0.06mm。
  10. 根据权利要求8所述的水性聚氨酯避孕套，其特征在于：所述水性聚氨酯避孕套包括以下特征中的任意一项或多项：
    100％拉伸模量小于等于2.0MPa；
    ***体积大于等于12升；
    ***压力大于等于1KPa；
    断裂延伸率大于等于650％；
    拉伸强度大于等于20MPa。
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