CN113201123A - 一种远红外共聚酯的制备方法 - Google Patents
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Abstract
本发明涉及聚酯材料领域,本发明公开了一种远红外共聚酯的制备方法,包括:将纳米级电气石粉和纳米级硼化铬粉、硬脂酸锌、γ‑脲基丙基三乙氧基硅烷混合研磨处理,加入到乙二醇和丁二醇的混合溶剂中,搅拌,超声分散,得到远红外功能复合醇溶液;(2)将远红外功能复合醇溶液与对苯二甲酸混合,加入缩聚催化剂,边打浆边加热搅拌,待温度达到230~250℃、压力为0.15~0.3MPa时进行酯化反应,常压升温至釜内温度280~290℃后开始抽真空,进行缩聚反应,出料切粒,制得远红外功能共聚酯。该功能聚酯可用作纤维、塑料、薄膜等产品的制备,广泛应用于远红外保健功能领域。
Description
技术领域
本发明涉及聚酯材料领域,尤其涉及一种远红外共聚酯的制备方法。
背景技术
共聚酯,由多元醇和多元酸缩聚而得的聚合物总称,是一类性能优异、用途广泛的工程塑料。也可制成聚酯纤维和聚酯薄膜。聚酯包括聚酯树脂和聚酯弹性体。纤维级聚酯切片用于制造涤纶短纤维和涤纶长丝,是供给涤纶纤维企业加工纤维及相关产品的原料,涤纶作为化纤中产量最大的品种,占据着化纤行业近80%的市场份额,因此聚酯系列的市场变化和发展趋势是化纤行业关注的重点。
随着人们对于纤维功能化需求的增长,越来越多的功能性纤维逐渐被开发出来,远红外纤维通常是在聚酯纤维中添加具有远红外功能的远红外添加剂。例如纳米级电气石粉和纳米级硼化铬粉等就具有出色的远红外效果,可起到远红外发热、释放负氧离子等保健功效。然而,目前较为传统的添加方式是在制得聚酯后将远红外添加剂在聚酯熔融或纺丝过程中进行复合,由于无机远红外添加剂与有机聚合物之间的相容性问题,导致无机远红外添加剂分散性较差、容易团聚,从而影响其功能发挥。
发明内容
为了解决上述技术问题,本发明提供了一种远红外共聚酯的制备方法。本发明先将具有远红外保健功能的纳米级电气石粉和纳米级硼化铬粉与硬脂酸锌、γ-脲基丙基三乙氧基硅烷混合研磨处理,进行表面改性,使其能够在共聚酯基体中相容性更好。且相较于传统的挤出共混等方式,本发明将无机远红外添加剂在共聚酯合成前的醇液中就进行添加,该方式能够使得无机远红外添加剂在聚合过程中就充分与聚合物分散、融合,相容性、分散性更佳。
本发明的具体技术方案为:一种远红外共聚酯的制备方法,包括以下步骤:
(1)按质量比(1~9):(9~1)将纳米级电气石粉和纳米级硼化铬粉混合加入至研钵中,再加入混合粉体总质量1~3%的硬脂酸锌、混合粉体总质量2~4%的γ-脲基丙基三乙氧基硅烷,研磨处理后,按质量比1~5%加入到乙二醇和丁二醇的混合溶剂中,搅拌,然后超声分散处理,得到远红外功能复合醇溶液。
(2)将远红外功能复合醇溶液与对苯二甲酸按(1.7~1.3):1的醇酸摩尔比混合,按对苯二甲酸质量的2~4‰加入缩聚催化剂,边打浆边加热搅拌,待温度达到230~250℃、压力为0.15~0.3MPa时进行酯化反应,常压升温至釜内温度280~290℃后开始抽真空,进行缩聚反应,出料切粒,制得远红外功能共聚酯。
作为优选,所述远红外功能共聚酯的特性黏度为0.60~0.64dL/g。
作为优选,步骤(1)中,研磨处理时间为2~4h。
作为优选,步骤(1)中,乙二醇和丁二醇的摩尔比为(95~85):(5~15)。
作为优选,步骤(1)中,搅拌0.5-1.5h,超声分散处理2~3h。
作为优选,步骤(2)中,所述缩聚催化剂为乙二醇锑。
作为优选,步骤(2)中,边打浆边加热搅拌2~3h。
作为优选,步骤(2)中,酯化反应2.5~3.5h。
作为优选,步骤(2)中,缩聚反应1.5~3h。
作为优选,步骤(2)中,在真空度100Pa以内进行缩聚反应。
与现有技术相比,本发明具有以下技术效果:本发明先将具有远红外保健功能的纳米级电气石粉和纳米级硼化铬粉与硬脂酸锌、γ-脲基丙基三乙氧基硅烷混合研磨处理,进行表面改性,使其能够在共聚酯基体中相容性更好。且相较于传统的挤出共混等方式,本发明将无机远红外添加剂在共聚酯合成前的醇液中就进行添加,该方式能够使得无机远红外添加剂在聚合过程中就充分与聚合物分散、融合,相容性、分散性更佳。本发明员工外共聚酯可用作纤维、塑料、薄膜等产品的制备,广泛应用于需要远红外保健功能的领域。
具体实施方式
下面结合实施例对本发明作进一步的描述。
实施例1
(1)按质量比1:9的比例将竹炭粉和碳化硅粉混合,再加入混合粉体质量1%的硬脂酸锌、混合粉体质量3.5%的乙烯基三甲氧基硅烷进行研磨处理3小时后,按照质量比2%的比例加入到摩尔比为90:10的乙二醇和丙二醇的混合溶剂中,用电动搅拌桨搅拌1小时,然后置于超声波中分散处理2.5小时,得到远红外功能复合醇溶液;
(2)将远红外功能复合醇溶液与对苯二甲酸按1.6:1的醇酸摩尔比的原料配比,按对苯二甲酸质量的3.5‰加入缩聚催化剂乙二醇锑,边打浆边加热搅拌2小时,待温度达到230℃、压力0.2MPa时酯化反应2.5小时后,常压升温至釜内温度283℃后开始抽真空,在真空度100Pa以内进行缩聚反应2.5小时,达到预定功率后出料切粒,制得远红外功能共聚酯.
上述过程制得的远红外共聚酯的特性黏度值在0.620dL/g,熔点为251℃。
实施例2
(1)按质量比1:1的比例将竹炭粉和碳化硅粉混合,再加入混合粉体质量2%的硬脂酸锌、混合粉体质量3%的乙烯基三甲氧基硅烷进行研磨处理3小时后,按照质量比2.5%的比例加入到摩尔比为80:20的乙二醇和丙二醇的混合溶剂中,用电动搅拌桨搅拌1小时,然后置于超声波中分散处理2.5小时,得到远红外功能复合醇溶液;
(2)将远红外功能复合醇溶液与对苯二甲酸按1.6:1的醇酸摩尔比的原料配比,按对苯二甲酸质量的3.5‰加入缩聚催化剂乙二醇锑,边打浆边加热搅拌2小时,待温度达到235℃、压力0.2MPa时酯化反应2.5小时后,常压升温至釜内温度284℃后开始抽真空,在真空度100Pa以内进行缩聚反应2.7小时,达到预定功率后出料切粒,制得远红外功能共聚酯.
上述过程制得的远红外共聚酯的特性黏度值在0.625dL/g,熔点为253℃。
实施例3
(1)按质量比7:3的比例将竹炭粉和碳化硅粉混合,再加入混合粉体质量2.5%的硬脂酸锌、混合粉体质量2.5%的乙烯基三甲氧基硅烷进行研磨处理3小时后,按照质量比3%的比例加入到摩尔比为50:50的乙二醇和丙二醇的混合溶剂中,用电动搅拌桨搅拌1小时,然后置于超声波中分散处理2.5小时,得到远红外功能复合醇溶液;
(2)将远红外功能复合醇溶液与对苯二甲酸按1.6:1的醇酸摩尔比的原料配比,按对苯二甲酸质量的3.5‰加入缩聚催化剂乙二醇锑,边打浆边加热搅拌2小时,待温度达到233℃、压力0.25MPa时酯化反应2.5小时后,常压升温至釜内温度284℃后开始抽真空,在真空度100Pa以内进行缩聚反应3小时,达到预定功率后出料切粒,制得远红外功能共聚酯.
上述过程制得的远红外共聚酯的特性黏度值在0.649dL/g,熔点为248℃。
本发明中所用原料、设备,若无特别说明,均为本领域的常用原料、设备;本发明中所用方法,若无特别说明,均为本领域的常规方法。
以上所述,仅是本发明的较佳实施例,并非对本发明作任何限制,凡是根据本发明技术实质对以上实施例所作的任何简单修改、变更以及等效变换,均仍属于本发明技术方案的保护范围。
Claims (10)
1.一种远红外共聚酯的制备方法,其特征在于:包括以下步骤:
(1)按质量比(1~9):(9~1)将纳米级电气石粉和纳米级硼化铬粉混合加入至研钵中,再加入混合粉体总质量1~3%的硬脂酸锌、混合粉体总质量2~4%的γ-脲基丙基三乙氧基硅烷,研磨处理后,按质量比1~5%加入到乙二醇和丁二醇的混合溶剂中,搅拌,然后超声分散处理,得到远红外功能复合醇溶液;
(2)将远红外功能复合醇溶液与对苯二甲酸按(1.7~1.3):1的醇酸摩尔比混合,按对苯二甲酸质量的2~4‰加入缩聚催化剂,边打浆边加热搅拌,待温度达到230~250℃、压力为0.15~0.3MPa时进行酯化反应,常压升温至釜内温度280~290℃后开始抽真空,进行缩聚反应,出料切粒,制得远红外功能共聚酯。
2.如权利要求1所述的制备方法,其特征在于:所述远红外功能共聚酯的特性黏度为0.60~0.64dL/g。
3.如权利要求1所述的制备方法,其特征在于:步骤(1)中,研磨处理时间为2~4h。
4.如权利要求1所述的制备方法,其特征在于:步骤(1)中,乙二醇和丁二醇的摩尔比为(95~85):(5~15)。
5.如权利要求1所述的制备方法,其特征在于:步骤(1)中,搅拌0.5-1.5h,超声分散处理2~3h。
6.如权利要求1所述的制备方法,其特征在于:步骤(2)中,所述缩聚催化剂为乙二醇锑。
7.如权利要求1所述的制备方法,其特征在于:步骤(2)中,边打浆边加热搅拌2~3h。
8.如权利要求1所述的制备方法,其特征在于:步骤(2)中,酯化反应2.5~3.5h。
9.如权利要求1所述的制备方法,其特征在于:步骤(2)中,缩聚反应1.5~3h。
10.如权利要求1所述的制备方法,其特征在于:步骤(2)中,在真空度100Pa以内进行缩聚反应。
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CN104988594A (zh) * | 2015-01-16 | 2015-10-21 | 浙江真北纺织新材料研究院有限公司 | 释放负离子、远红外及阻燃复合功能聚酯纤维的制备方法 |
CN109295532A (zh) * | 2018-09-29 | 2019-02-01 | 浙江和也健康科技有限公司 | 一种抗菌复合型功能纤维及其制备方法 |
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CN104988594A (zh) * | 2015-01-16 | 2015-10-21 | 浙江真北纺织新材料研究院有限公司 | 释放负离子、远红外及阻燃复合功能聚酯纤维的制备方法 |
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