CN106883377A - 一种利用生产tmpta废水制备的固化剂及其方法 - Google Patents
一种利用生产tmpta废水制备的固化剂及其方法 Download PDFInfo
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Abstract
本发明公开了一种利用生产TMPTA废水制备的固化剂,包含如下重量组份的各物质:TMPTA工业废水50‑80份、4‑乙酰氨基水杨酸10‑15份、L‑半胱氨酸3‑8份、水杨酸‑2‑乙基己基酯8‑12份、乙酸乙酯6‑10份、5‑硝基糠醛二乙酸酯9‑14份、2‑噻吩甲醛3‑6份、丁香酚4‑8份、5‑羟基色胺2‑5份、二巯丙醇7‑12份。本发明将三羟甲基丙烷三丙烯酸酯(TMPTA)的生产废水经简单浓缩后,加入多种有机化学成分,制备成性能优良的固化剂。
Description
技术领域
本发明属于TMPTA废水处理领域,特别涉及一种利用生产TMPTA废水制备的固化剂及其方法。
背景技术
三羟甲基丙烷三丙烯酸酯 (TMPTA) 是一种重要的化工原料,主要用于制造光固化涂料、光固化油墨、光刻胶、柔性印刷品、阻焊剂、抗蚀剂、油漆和聚合物改性等。在生产三羟甲基丙烷三丙烯酸酯 (TMPTA) 时产生大量的废水严重污染环境。现有技术中,三羟甲基丙烷三丙烯酸酯 (TMPTA) 生产厂家都是把废水蒸发浓缩得到一种没有任何价值、在土壤中不能分解的固形物,运到“偏僻”地区填埋,非常造成二次污染;浓缩时需要消耗大量能源,处理成本极高。并且三羟甲基丙烷三丙烯酸酯 (TMPTA) 的生产废水中含有大量的丙烯酸和丙烯酸钠,而丙烯酸和丙烯酸钠是重要的化工原材料,单一的浓缩填埋造成了极大的浪费。
固化剂又名硬化剂、熟化剂或变定剂,是一类增进或控制固化反应的物质或混合物。树脂固化是经过缩合、闭环、加成或催化等化学反应,使热固性树脂发生不可逆的变化过程,固化是通过添加固化(交联)剂来完成的。固化剂是必不可少的添加物,无论是作粘接剂、涂料、浇注料都需添加固化剂,否则环氧树脂不能固化。固化剂的品种对固化物的力学性能、耐热性、耐水性、耐腐蚀性等都有很大影响。因此,将三羟甲基丙烷三丙烯酸酯(TMPTA) 的生产废水制备成固化剂有其现实意义。
发明内容
针对上述缺陷,本发明的目的是提供一种利用生产TMPTA废水制备的固化剂及其方法,将三羟甲基丙烷三丙烯酸酯 (TMPTA) 的生产废水经简单浓缩后,加入多种有机化学成分,制备成性能优良的固化剂。
本发明的目的可以通过以下技术方案实现:
一种利用生产TMPTA废水制备的固化剂,包含如下重量组份的各物质:TMPTA工业废水50-80份、4-乙酰氨基水杨酸10-15份、L-半胱氨酸3-8份、水杨酸-2-乙基己基酯8-12份、乙酸乙酯6-10份、5-硝基糠醛二乙酸酯9-14份、2-噻吩甲醛3-6份、丁香酚4-8份、5-羟基色胺2-5份、二巯丙醇7-12份。
优选的,所述TMPTA工业废水60-70份、4-乙酰氨基水杨酸11-14份、L-半胱氨酸4-7份、水杨酸-2-乙基己基酯9-11份、乙酸乙酯7-9份、5-硝基糠醛二乙酸酯10-12份、2-噻吩甲醛4-6份、丁香酚5-8份、5-羟基色胺3-5份、二巯丙醇8-11份。
优选的,所述TMPTA工业废水65份、4-乙酰氨基水杨酸12份、L-半胱氨酸6份、水杨酸-2-乙基己基酯10份、乙酸乙酯8份、5-硝基糠醛二乙酸酯11份、2-噻吩甲醛5份、丁香酚6份、5-羟基色胺4份、二巯丙醇10份。
一种利用生产TMPTA废水制备固化剂的方法,包括如下步骤:
S1:将TMPTA工业废水50-80份减压蒸发浓缩至丙烯酸钠含量大于30%的丙烯酸钠浓缩液;
S2:向步骤S1中加入4-乙酰氨基水杨酸10-15份、L-半胱氨酸3-8份、水杨酸-2-乙基己基酯8-12份、乙酸乙酯6-10份,升高温度至60-80℃,保温反应20-40min;
S3:向步骤S2中加入5-硝基糠醛二乙酸酯9-14份、2-噻吩甲醛3-6份、二巯丙醇7-12份,继续升高温度至80-110℃,以速率800-1200r/min搅拌反应1-2h;
S4:向步骤S3中加入5-羟基色胺2-5份、丁香酚4-8份,搅拌5-15min后,微波加热反应20-30min;待反应冷却后即可得到所述固化剂。
优选的,步骤S1中所述减压蒸发浓缩至丙烯酸钠含量为45%的丙烯酸钠浓缩液。
优选的,步骤S2中所述温度为72℃,保温反应35min。
优选的,步骤S3中所述温度为100℃,速率为1000r/min,搅拌反应1.5h。
优选的,步骤S4中搅拌8min,微波功率为3500W,微波加热反应25min。
本发明与现有技术相比,其有益效果为:
本发明所述一种利用生产TMPTA废水制备固化剂的方法,利用含有大量的丙烯酸和丙烯酸钠的三羟甲基丙烷三丙烯酸酯 (TMPTA) 的生产废水,并且在原有固化剂配方基础上加入5-硝基糠醛二乙酸酯、丁香酚、5-羟基色胺、二巯丙醇等化学成分,制备成综合性能优良的固化剂。该固化剂的耐碱性为350-480s,拉伸强度为25-35Mpa,冲击强度为110-120KJ/m2。
具体实施方式
以下结合实施例对本发明作进一步的说明。
实施例1
S1:将TMPTA工业废水50份减压蒸发浓缩至丙烯酸钠含量35%的丙烯酸钠浓缩液;
S2:向步骤S1中加入4-乙酰氨基水杨酸10份、L-半胱氨酸3份、水杨酸-2-乙基己基酯8份、乙酸乙酯6份,升高温度至60℃,保温反应20min;
S3:向步骤S2中加入5-硝基糠醛二乙酸酯9份、2-噻吩甲醛3份、二巯丙醇7份,继续升高温度至80℃,以速率800r/min搅拌反应1h;
S4:向步骤S3中加入5-羟基色胺2份、丁香酚4份,搅拌5min后,在功率3500W下微波加热反应20min;待反应冷却后即可得到所述固化剂。
对比例1
S1:将TMPTA工业废水50份减压蒸发浓缩至丙烯酸钠含量35%的丙烯酸钠浓缩液;
S2:向步骤S1中加入4-乙酰氨基水杨酸10份、L-半胱氨酸3份、水杨酸-2-乙基己基酯8份、乙酸乙酯6份,升高温度至60℃,保温反应20min;
S3:向步骤S2中加入2-噻吩甲醛3份,继续升高温度至80℃,以速率800r/min搅拌反应1h;在功率3500W下微波加热反应20min;待反应冷却后即可得到所述固化剂。
实施例2
S1:将TMPTA工业废水80份减压蒸发浓缩至丙烯酸钠含量55%的丙烯酸钠浓缩液;
S2:向步骤S1中加入4-乙酰氨基水杨酸15份、L-半胱氨酸8份、水杨酸-2-乙基己基酯12份、乙酸乙酯10份,升高温度至80℃,保温反应40min;
S3:向步骤S2中加入5-硝基糠醛二乙酸酯14份、2-噻吩甲醛6份、二巯丙醇12份,继续升高温度至110℃,以速率1200r/min搅拌反应2h;
S4:向步骤S3中加入5-羟基色胺5份、丁香酚8份,搅拌15min后,在功率3500W下微波加热反应30min;待反应冷却后即可得到所述固化剂。
对比例2
S1:将TMPTA工业废水80份减压蒸发浓缩至丙烯酸钠含量55%的丙烯酸钠浓缩液;
S2:向步骤S1中加入4-乙酰氨基水杨酸15份、L-半胱氨酸8份、水杨酸-2-乙基己基酯12份、乙酸乙酯10份,升高温度至80℃,保温反应40min;
S3:向步骤S2中加入2-噻吩甲醛6份,继续升高温度至110℃,以速率1200r/min搅拌反应2h;在功率3500W下微波加热反应30min;待反应冷却后即可得到所述固化剂。
实施例3
S1:将TMPTA工业废水60份减压蒸发浓缩至丙烯酸钠含量35%的丙烯酸钠浓缩液;
S2:向步骤S1中加入4-乙酰氨基水杨酸11份、L-半胱氨酸4份、水杨酸-2-乙基己基酯9份、乙酸乙酯7份,升高温度至60℃,保温反应40min;
S3:向步骤S2中加入5-硝基糠醛二乙酸酯10份、2-噻吩甲醛4份、二巯丙醇8份,继续升高温度至90℃,以速率800r/min搅拌反应2h;
S4:向步骤S3中加入5-羟基色胺3份、丁香酚5份,搅拌10min后,在功率3500W下微波加热反应30min;待反应冷却后即可得到所述固化剂。
实施例4
S1:将TMPTA工业废水70份减压蒸发浓缩至丙烯酸钠含量55%的丙烯酸钠浓缩液;
S2:向步骤S1中加入4-乙酰氨基水杨酸14份、L-半胱氨酸7份、水杨酸-2-乙基己基酯11份、乙酸乙酯9份,升高温度至80℃,保温反应20min;
S3:向步骤S2中加入5-硝基糠醛二乙酸酯12份、2-噻吩甲醛6份、二巯丙醇11份,继续升高温度至100℃,以速率1000r/min搅拌反应1h;
S4:向步骤S3中加入5-羟基色胺5份、丁香酚8份,搅拌5min后,在功率3500W下微波加热反应20min;待反应冷却后即可得到所述固化剂。
实施例5
S1:将TMPTA工业废水65份减压蒸发浓缩至丙烯酸钠含量45%的丙烯酸钠浓缩液;
S2:向步骤S1中加入4-乙酰氨基水杨酸12份、L-半胱氨酸6份、水杨酸-2-乙基己基酯10份、乙酸乙酯8份,升高温度至72℃,保温反应35min;
S3:向步骤S2中加入5-硝基糠醛二乙酸酯11份、2-噻吩甲醛5份、二巯丙醇10份,继续升高温度至100℃,以速率1000r/min搅拌反应1.5h;
S4:向步骤S3中加入5-羟基色胺4份、丁香酚6份,搅拌5min后,在功率3500W下微波加热反应25min;待反应冷却后即可得到所述固化剂。
将上述各个实施例和对比例所得固化剂进行性能测试,结果如下:
试验 | 耐碱性/s | 拉伸强度/Mpa | |
实施例1 | 350 | 25 | 110 |
对比例1 | 108 | 13 | 82 |
实施例2 | 370 | 28 | 112 |
对比例2 | 120 | 10 | 87 |
实施例3 | 400 | 30 | 115 |
实施例4 | 450 | 32 | 117 |
实施例5 | 480 | 35 | 120 |
本发明不限于这里的实施例,本领域技术人员根据本发明的揭示,不脱离本发明范畴所做出的改进和修改都应该在本发明的保护范围之内。
Claims (8)
1.一种利用生产TMPTA废水制备的固化剂,其特征在于,包含如下重量组份的各物质:
TMPTA工业废水50-80份、4-乙酰氨基水杨酸10-15份、L-半胱氨酸3-8份、水杨酸-2-乙基己基酯8-12份、乙酸乙酯6-10份、5-硝基糠醛二乙酸酯9-14份、2-噻吩甲醛3-6份、丁香酚4-8份、5-羟基色胺2-5份、二巯丙醇7-12份。
2.根据权利要求1所述的一种利用生产TMPTA废水制备的固化剂,其特征在于,所述TMPTA工业废水60-70份、4-乙酰氨基水杨酸11-14份、L-半胱氨酸4-7份、水杨酸-2-乙基己基酯9-11份、乙酸乙酯7-9份、5-硝基糠醛二乙酸酯10-12份、2-噻吩甲醛4-6份、丁香酚5-8份、5-羟基色胺3-5份、二巯丙醇8-11份。
3.根据权利要求2所述的一种利用生产TMPTA废水制备的固化剂,其特征在于,所述TMPTA工业废水65份、4-乙酰氨基水杨酸12份、L-半胱氨酸6份、水杨酸-2-乙基己基酯10份、乙酸乙酯8份、5-硝基糠醛二乙酸酯11份、2-噻吩甲醛5份、丁香酚6份、5-羟基色胺4份、二巯丙醇10份。
4.一种利用生产TMPTA废水制备固化剂的方法,其特征在于,包括如下步骤:
S1:将TMPTA工业废水50-80份减压蒸发浓缩至丙烯酸钠含量大于30%的丙烯酸钠浓缩液;
S2:向步骤S1中加入4-乙酰氨基水杨酸10-15份、L-半胱氨酸3-8份、水杨酸-2-乙基己基酯8-12份、乙酸乙酯6-10份,升高温度至60-80℃,保温反应20-40min;
S3:向步骤S2中加入5-硝基糠醛二乙酸酯9-14份、2-噻吩甲醛3-6份、二巯丙醇7-12份,继续升高温度至80-110℃,以速率800-1200r/min搅拌反应1-2h;
S4:向步骤S3中加入5-羟基色胺2-5份、丁香酚4-8份,搅拌5-15min后,微波加热反应20-30min;待反应冷却后即可得到所述固化剂。
5.根据权利要求4所述的一种利用生产TMPTA废水制备固化剂的方法,其特征在于,步骤S1中所述减压蒸发浓缩至丙烯酸钠含量为45%的丙烯酸钠浓缩液。
6.根据权利要求4所述的一种利用生产TMPTA废水制备固化剂的方法,其特征在于,步骤S2中所述温度为72℃,保温反应35min。
7.根据权利要求4所述的一种利用生产TMPTA废水制备固化剂的方法,其特征在于,步骤S3中所述温度为100℃,速率为1000r/min,搅拌反应1.5h。
8.根据权利要求4所述的一种利用生产TMPTA废水制备固化剂的方法,其特征在于,步骤S4中搅拌8min,微波功率为3500W,微波加热反应25min。
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