WO2021163848A1 - 一种非多孔性球形二氧化硅开口剂的制备方法、由此得到的薄膜开口剂及其应用 - Google Patents

一种非多孔性球形二氧化硅开口剂的制备方法、由此得到的薄膜开口剂及其应用 Download PDF

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WO2021163848A1
WO2021163848A1 PCT/CN2020/075560 CN2020075560W WO2021163848A1 WO 2021163848 A1 WO2021163848 A1 WO 2021163848A1 CN 2020075560 W CN2020075560 W CN 2020075560W WO 2021163848 A1 WO2021163848 A1 WO 2021163848A1
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preparation
blocking agent
opening agent
porous spherical
agent
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PCT/CN2020/075560
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English (en)
French (fr)
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陈树真
李锐
唐成
丁烈平
陈晨
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浙江三时纪新材科技有限公司
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Priority to CN202080001771.6A priority Critical patent/CN112384475B/zh
Priority to PCT/CN2020/075560 priority patent/WO2021163848A1/zh
Publication of WO2021163848A1 publication Critical patent/WO2021163848A1/zh

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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/113—Silicon oxides; Hydrates thereof
    • C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
    • 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
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/34—Silicon-containing compounds
    • C08K3/36—Silica
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
    • C08L83/04—Polysiloxanes
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
    • C08L83/04—Polysiloxanes
    • C08L83/06—Polysiloxanes containing silicon bound to oxygen-containing groups
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
    • C08L83/04—Polysiloxanes
    • C08L83/08—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen

Definitions

  • the present invention relates to a film opening agent, and more specifically to a preparation method of a non-porous spherical silica opening agent, a film opening agent obtained therefrom, and applications thereof.
  • the film opening agent is a small amount of inorganic particles that are added to the plastic film to form bumps on the surface of the film to make the film difficult to adhere and peel off.
  • the most commonly used is silica.
  • the opening agent requires no coarse particles, because the coarse particles will fall off and cause scratches on the film.
  • the opening agent requires no fine powder, because the fine powder does not function as an opening agent and will affect the transparency of the film. Since the film thickness of the film is generally 10 to 50 microns, the average diameter of the anti-blocking agent is 0.5 to 5 microns.
  • the current antiblocking agents are silica particles with a narrow particle size distribution with an average diameter of 0.5 to 5 microns, and the most commonly used are granulated products of wet-process silica.
  • the current opening agent is generally porous particles, which will reduce the gas barrier properties of the film, and is not suitable for film products that require air tightness.
  • the present invention provides a method for preparing a non-porous spherical silica opening agent. Film opening agent and its application.
  • a method for preparing a non-porous spherical silica opening agent which includes the following steps: S1, a spherical polysiloxane comprising T units is provided by the hydrolysis condensation reaction of hydrocarbyl trialkoxysilane, Among them, the unit of T is R 1 SiO 3 -, R 1 is a hydrogen atom or an independently selectable organic group with carbon atoms of 1 to 18; S2, spherical polysiloxane is calcined in an oxidizing gas atmosphere, and the calcining temperature is 450 Between degrees and 1200 degrees, a non-porous spherical silica opening agent that does not contain silica particles with a diameter greater than 10 microns is obtained.
  • the step S1 includes: hydrolyzing the hydrocarbyl trialkoxysilane under acidic conditions to dissolve in deionized water, and then condensing under alkaline conditions to obtain spherical polysiloxane.
  • the hydrocarbyl trialkoxysilane is methyltrimethoxysilane.
  • the step S1 is specifically: adding deionized water into a reactor with a stirrer, adding hydrocarbyl trialkoxysilane and acetic acid under stirring, adding ammonia water, stirring, standing, filtering, and drying to obtain Spherical polysiloxane.
  • the weight ratio of deionized water and hydrocarbyl trialkoxysilane is 750-1800:80.
  • the ammonia water is 5% by mass dilute ammonia water.
  • the weight ratio of deionized water to ammonia water is 750-1800:25.
  • the oxidizing gas contains oxygen to oxidize all the organic substances in the polysiloxane.
  • the step S2 includes: putting the spherical polysiloxane powder into a muffle furnace and passing dry air into it for calcination.
  • the calcination temperature is between 450 degrees and 1100 degrees, and the calcination time is between 6 hours and 12 hours.
  • the preparation method further includes adding a treatment agent to perform surface treatment on the spherical silica powder filler, the treatment agent including a silane coupling agent and/or disilazane;
  • the silane coupling agent is (R 7 ) a (R 8 ) b Si(M) 4-ab
  • the present invention also provides a film opening agent obtained according to the above preparation method, which does not contain silica particles with a diameter greater than 10 microns, and the average particle size of the non-porous spherical silica opening agent is between 0.5 microns and 5 microns between. More preferably, the average particle size of the non-porous spherical silica opening agent is between 0.5 ⁇ m and 4 ⁇ m.
  • the present invention also provides an application of the above-mentioned film opening agent.
  • the above-mentioned non-porous spherical silica opening agent and an organic resin are mixed to form a master batch suitable for film.
  • the provided silica particles have no porosity and will not cause a decrease in gas barrier properties, and are suitable for thin film products with air tightness requirements.
  • the film opening agent according to the present invention has high film gas barrier properties, high transparency and high opening release properties.
  • the average particle size is measured with HORIBA's LA-700 laser particle size distribution analyzer
  • the blocking agent of the comparative example, Sylobloc45 from W. RGrace Company, and the blocking agent of the embodiment of the present invention were added to the polypropylene raw material at an added amount of 0.1% and mixed and then blown into a film with a film thickness of 20 microns.
  • the opening property was evaluated with a commercially available film opening property tester.
  • oxygen permeability the low-pressure and high-pressure chambers are separated by a thin film sample, and the high-pressure chamber is filled with 105 Pa of oxygen. The low-pressure chamber is evacuated, and then the pressure increase in the low-pressure chamber after a certain period of time is measured.
  • the average particle size refers to the volume average diameter of the particles.
  • Example 3 The spherical silica of Example 3 was treated with vinyl trimethoxysilane to obtain the spherical silica of Example 5.

Abstract

一种非多孔性球形二氧化硅开口剂的制备方法，其具有如下步骤：S1，由烃基三烷氧基硅烷的加水分解缩合反应来提供包括T单位的球形聚硅氧烷，其中，T单位为R1SiO 3-，R1为氢原子或可独立选择的碳原子1至18的有机基；S2，在氧化气体氛围条件下煅烧球形聚硅氧烷，煅烧温度介于450度-1200度之间，得到不含有直径大于10微米的二氧化硅粒子的非多孔性球形二氧化硅开口剂。一种根据上述的制备方法得到的薄膜开口剂。一种上述的薄膜开口剂的应用。该薄膜开口剂具有高薄膜气体屏障性，高透明性和高开口防粘性。

Description

一种非多孔性球形二氧化硅开口剂的制备方法、由此得到的薄膜开口剂及其应用 技术领域
本发明涉及薄膜开口剂，更具体地涉及一种非多孔性球形二氧化硅开口剂的制备方法、由此得到的薄膜开口剂及其应用。
背景技术
薄膜开口剂是少量添加在塑料薄膜中，在膜表面形成凸起使薄膜不易粘接、易剥离的无机粒子，其中最常用的是二氧化硅。开口剂要求不能存在粗大颗粒，因为粗大颗粒会脱落并在薄膜上产生划痕。同时开口剂要求不存在细粉，因为细粉不起开口剂作用，且会影响薄膜的透明性。由于薄膜的膜厚一般在10至50微米，开口剂的平均直径在0.5至5微米。因此，现在的开口剂是平均直径0.5至5微米的粒度分布狭的二氧化硅粒子，最常用的是湿法二氧化硅的造粒品。但现在的开口剂一般为多孔性粒子，会造成薄膜的气体屏障性下降，不适于有气密性要求的薄膜产品。
发明内容
为了解决上述现有技术中的薄膜开口剂为多孔性粒子而不适用于有气密性要求的薄膜的问题，本发明提供一种非多孔性球形二氧化硅开口剂的制备方法、由此得到的薄膜开口剂及其应用。
根据本发明提供一种非多孔性球形二氧化硅开口剂的制备方法，其包括如下步骤：S1，由烃基三烷氧基硅烷的加水分解缩合反应来提供包括T单位的球形聚硅氧烷，其中，T单位为R 1SiO 3-，R 1为氢原子或可独立选择的碳原子1至18的有机基；S2，在氧化气体氛围条件下煅烧球形聚硅氧烷，煅烧温度介于450度-1200度之间，得到不含有直径大于10微米的二氧化硅粒子的非多孔性球形二氧化硅开口剂。
优选地，所述步骤S1包括：将烃基三烷氧基硅烷在酸性条件下加水分解溶于去离子水中，然后在碱性条件下缩合得球形聚硅氧烷。在优选的实施例中，烃基三烷氧基硅烷为甲基三甲氧基硅烷。
优选地，所述步骤S1具体为：将去离子水加入带有搅拌器的反应釜内，在搅拌的情况下加入烃基三烷氧基硅烷和醋酸，加入氨水搅拌后静置，过滤，干燥得球形聚硅氧烷。
优选地，去离子水和烃基三烷氧基硅烷的重量比为750-1800：80。
优选地，氨水为质量百分比5％的稀氨水。
优选地，去离子水和氨水的重量比为750-1800：25。
优选地，氧化气体中含有氧气以将聚硅氧烷中的有机物全部氧化。具体地，所述步骤S2包括：将球形聚硅氧烷粉体放入马弗炉中通入干燥空气进行煅烧。
优选地，煅烧温度介于450度-1100度之间，煅烧时间介于6小时-12小时之间。
优选地，该球形聚硅氧烷还含有Q单位、D单位、和/或M单位，其中，Q单位＝SiO 4-，D单位＝R 2R 3SiO 2-，M单位＝R 4R 5R 6SiO 2-，R 2，R 3，R 4，R 5，R 6分别为氢原子或可独立选择的碳原子1至18的烃基。
优选地，该制备方法还包括加入处理剂对球形二氧化硅粉体填料进行表面处理，该处理剂包括硅烷偶联剂和/或二硅氮烷；该硅烷偶联剂为(R 7) a(R 8) bSi(M) 4-a-b，R 7，R 8为可独立选择的碳原子1至18的烃基、氢原子、或被官能团置换的碳原子1至18的烃基，该官能团选自由以下有机官能团组成的组中的至少一种：乙烯基，烯丙基，苯乙烯基，环氧基，脂肪族氨基，芳香族氨基，甲基丙烯酰氧丙基，丙烯酰氧丙基，脲基丙基，氯丙基，巯基丙基，聚硫化物基，异氰酸酯丙基；M为碳原子1至18的烃氧基或卤素原子，a＝0、1、2或3，b＝0、1、2或3，a+b＝1、2或3；该二硅氮烷为(R 9R 10R 11)SiNHSi(R 12R 13R 14)，R 9，R 10，R 11，R 12，R 13，R 14为可独立选择的碳原子1至18的烃基或氢原子。在一个优选的实施例中，该处理剂为乙烯基三甲氧基硅烷。
本发明还提供一种根据上述的制备方法得到的薄膜开口剂，其不含有直径大于10微米的二氧化硅粒子，非多孔性球形二氧化硅开口剂的平均粒径介于0.5微米-5微米之间。更优选地，非多孔性球形二氧化硅开口剂的平均粒径介于0.5微米-4微米之间。
本发明又提供一种上述的薄膜开口剂的应用，上述的非多孔性球形二氧化硅开口剂和有机树脂混合形成母料以适用于薄膜。
根据本发明的非多孔性球形二氧化硅开口剂的制备方法，提供的二氧化硅粒子不具有多孔性，不会导致气体屏障性下降，适用于气密性要求的薄膜产品。总之，根据本发明的薄膜开口剂具有高薄膜气体屏障性，高透明性和高开口防粘性。
具体实施方式
下面给出本发明的较佳实施例，并予以详细描述。
以下实施例中涉及的检测方法包括：
平均粒径用HORIBA的激光粒度分布仪LA-700测定；
10微米以上二氧化硅粒子的有无用场发射扫描电子显微(FE-SEM)镜直接观测，任意选择10张5千倍照片，以实质上观测不到10微米以上颗粒为不含10微米以上粗大颗粒粒子；
将对比例的开口剂、W.RGrace公司的Sylobloc45，本发明的实施例开口剂按0.1％的添加量添加到聚丙烯原料中混合后吹膜，膜厚20微米。开口性用市贩薄膜开口性测试仪评价。氧气透过性用薄膜试样将低压和高压室隔开，高压室充105Pa的氧气。低压室抽真空，然后测一定时间后的低压室的压力增量。以Sylocloc45为其准测出了实施例的相对氧气透过性，即：相对氧气透过量＝(实施例的压力增量/Sylobloc45的压力增量)×100；
在本文中，“度”指的是“摄氏度”，即℃。
在本文中，平均粒径指粒子的体积平均直径。
例1
室温下取一定重量部的去离子水放入带有搅拌器的反应釜内，开启搅拌，加入80重量部的甲基三甲氧基硅烷和少量醋酸将PH调至5左右。甲基三甲氧基硅烷溶解后加入25重量部5％的氨水搅拌10秒钟后停止搅拌。静止1小时后过滤，干燥后得球形聚硅氧烷。将聚硅氧烷粉体放入马弗炉中通入干燥空气进行煅烧，煅烧时间为12小时。样品的分析结果列入下表1。
表1
Figure PCTCN2020075560-appb-000001
例2
将实施例3的球形二氧化硅用乙烯基三甲氧基硅烷处理得实施例5的球形二氧化硅。
例3
Sylobloc45和实施例1至5的开口性、相对氧气透过性列于下表2。
表2
样品 开口性 相对氧气透过量(％)
Sylobloc45 易揭开 100
实施例1 可揭开 78
实施例2 易揭开 82
实施例3 易揭开 85
实施例4 易揭开 86
实施例5 易揭开 80
以上所述的，仅为本发明的较佳实施例，并非用以限定本发明的范围，本发明的上述实施例还可以做出各种变化。即凡是依据本发明申请的权利要求书及说明书内容所作的简单、等效变化与修饰，皆落入本发明专利的权利要求保护范围。本发明未详尽描述的均为常规技术内容。

Claims (9)

  1. 一种非多孔性球形二氧化硅开口剂的制备方法，其特征在于，该制备方法具有如下步骤：
    S1，由烃基三烷氧基硅烷的加水分解缩合反应来提供包括T单位的球形聚硅氧烷，其中，T单位为R 1SiO 3-，R 1为氢原子或可独立选择的碳原子1至18的有机基；
    S2，在氧化气体氛围条件下煅烧球形聚硅氧烷，煅烧温度介于450度-1200度之间，得到不含有直径大于10微米的二氧化硅粒子的非多孔性球形二氧化硅开口剂。
  2. 根据权利要求1所述的制备方法，其特征在于，所述步骤S1包括：将烃基三烷氧基硅烷在酸性条件下加水分解溶于去离子水中，然后在碱性条件下缩合得球形聚硅氧烷。
  3. 根据权利要求2所述的制备方法，其特征在于，所述步骤S1具体为：将去离子水加入带有搅拌器的反应釜内，在搅拌的情况下加入烃基三烷氧基硅烷和醋酸，加入氨水搅拌后静置，过滤，干燥得球形聚硅氧烷。
  4. 根据权利要求3所述的制备方法，其特征在于，去离子水和烃基三烷氧基硅烷的重量比为750-1800：80。
  5. 根据权利要求3所述的制备方法，其特征在于，去离子水和氨水的重量比为750-1800：25。
  6. 根据权利要求1所述的制备方法，其特征在于，该球形聚硅氧烷还含有Q单位、D单位、和/或M单位，其中，Q单位＝SiO 4-，D单位＝R 2R 3SiO 2-，M单位＝R 4R 5R 6SiO 2-，R 2，R 3，R 4，R 5，R 6分别为氢原子或可独立选择的碳原子1至18的烃基。
  7. 根据权利要求1所述的制备方法，其特征在于，该制备方法还包括加入处理剂对球形二氧化硅粉体填料进行表面处理，该处理剂包括硅烷偶联剂和/或二硅氮烷；该硅烷偶联剂为(R 7) a(R 8) bSi(M) 4-a-b，R 7，R 8为可独立选择的碳原子1至18的烃基、氢原子、或被官能团置换的碳原子1至18的烃基，该官能团选自由以下有机官能团组成的组中的至少一种：乙烯基，烯丙基，苯乙烯基，环氧基，脂肪族氨基，芳香族氨基，甲基丙烯酰氧丙基，丙烯酰氧丙基，脲基丙基，氯丙基，巯基丙基，聚硫化物基，异氰酸酯丙基；M为 碳原子1至18的烃氧基或卤素原子，a＝0、1、2或3，b＝0、1、2或3，a+b＝1、2或3；该二硅氮烷为(R 9R 10R 11)SiNHSi(R 12R 13R 14)，R 9，R 10，R 11，R 12，R 13，R 14为可独立选择的碳原子1至18的烃基或氢原子。
  8. 一种根据上述权利要求1-7中任一项所述的制备方法得到的薄膜开口剂，其特征在于，该非多孔性球形二氧化硅开口剂不含有直径大于10微米的二氧化硅粒子，非多孔性球形二氧化硅开口剂的平均粒径介于0.5微米-5微米之间。
  9. 一种根据权利要求8所述的薄膜开口剂的应用，其特征在于，非多孔性球形二氧化硅开口剂和有机树脂混合形成母料以适用于薄膜。
PCT/CN2020/075560 2020-02-17 2020-02-17 一种非多孔性球形二氧化硅开口剂的制备方法、由此得到的薄膜开口剂及其应用 WO2021163848A1 (zh)

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