CN102675773B - Soft poly vinyl chloride (PVC) plasticizer and preparation method thereof - Google Patents
Soft poly vinyl chloride (PVC) plasticizer and preparation method thereof Download PDFInfo
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- CN102675773B CN102675773B CN201210175998.XA CN201210175998A CN102675773B CN 102675773 B CN102675773 B CN 102675773B CN 201210175998 A CN201210175998 A CN 201210175998A CN 102675773 B CN102675773 B CN 102675773B
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Abstract
The invention discloses a soft poly vinyl chloride (PVC) plasticizer and a preparation method thereof. The method comprises enabling 1,3-diglycidyl-S-triazine triketone to serve as a raw material, adding diethylenetriamine, carbamide, isophorone diisocyanate (IPDI), an antioxidant and a catalyst, and obtaining the viscous plasticizer after oil bath heating and rotating distillation. The plasticizer prepared through the method is non-toxic, environment-friendly, good in compatibility with PVC resin, low in production cost, high in plasticization efficiency and good in durability and environment-friendliness.
Description
Technical field
The present invention relates to technical field of polymer materials, be specifically related to flexible PVC softening agent and preparation method thereof.
Background technology
Softening agent is the kind of output and consumption maximum in plastic industry processing aid, and its output accounts for 60% of additives for plastics total amount, is mainly used in polrvinyl chloride product, and consumption accounts for 80% of softening agent total amount.At present, the softening agent that China overwhelming majority's plastic cement enterprise is used is DOP (dioctyl phthalate (DOP)), DINP (diisononyl phthalate) and DBP (dibutyl phthalate) etc., and this class softening agent is also used in the soft goods such as PVC flexible pipe, leatheroid, film in a large number.Because some metal element content in softening agent exceeds standard, to say from the strict sense, they are not novel environment friendly materials, in many performances, particularly the aspect such as low toxicity, health is difficult to meet the demands.Studies confirm that, DOP can enter human body through number of ways such as respiratory tract, mouth, skin absorption, intravenous infusions. body is had to very large toxic action.In medicine equipment, the DOP of PVC goods is discharged in patient body, can produce larger harm to patient.Within 2005, European Union gives a warning: originate in Chinese nipple of feeding bottle and contain DOP, do not meet relevant hygienic standard, forbid selling.And for example, 2005 Nianl0Yue， State General Administration for Quality Supervision tissues have been spot-check 44 kinds of PVC food fresh keeping membranes. and wherein in 12 kinds of PVC fresh-preserving films, contain adipic acid ester, relevant departments have ordered the sale that stops dispatching from the factory of relevant enterprise.Softening agent is one of requisite auxiliary agent in flexible PVC goods, and makes a general survey of global Plastics Industry, and PVC is the resin that annual production is only second to polyethylene (PE).Along with the development of plastics industry, the demand of softening agent increases year by year, and in order to address the above problem, the sector attempts to find a kind of novel substitute.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of flexible PVC softening agent, and this softening agent is nontoxic, environmental protection, can meet service requirements, and the present invention also will provide the preparation method of this softening agent simultaneously.
The present invention is achieved through the following technical solutions:
A softening agent, is comprised of following raw materials in part by weight:
1,3-2-glycidyl-S-triazinetrione 100, diethylenetriamine 2-6, carbonyl diamine 1-5, isophorone diisocyanate (IPDI) 0.1-1, antioxidant 0.01-0.3, catalyzer 0.01-1.15.
The further improvement project of the present invention is, described catalyzer is a kind of, two or more mixture in dibutyl tin laurate, stannous octoate or tetrabutyl titanate (can arbitrary proportion mix).
The further improvement project of the present invention is, described antioxidant is a kind of, two or more mixture in antioxidant AT215, antioxidant DSTDP or four (β-(tri-grades of butyl-4-hydroxy phenyls of 3,5-) propionic acid) pentaerythritol ester (can arbitrary proportion mix).
The method of preparing above-mentioned a kind of flexible PVC softening agent, comprises the following steps:
By above-mentioned proportioning, by 1, a kind of or two kinds of mixtures in 3-2-glycidyl-S-triazinetrione, Racemic glycidol-S-triazinetrione are put into 1000mL single port flask, add diethylenetriamine, carbonyl diamine, unlatching Rotary Evaporators heats up, (oil bath heating), speed is 2-5 ℃/min, stops after being then warming up to 60-80 ℃ heating up, and continues to stir 10-30min, then add isophorone diisocyanate, antioxidant, catalyzer, be warming up to 120-140 ℃, rotary distillation 2-5h, obtains finished product.
The present invention compared with prior art, has the following advantages:
Softening agent of the present invention is nontoxic, environmental protection, and good with polyvinyl chloride resin consistency, and speedup efficiency is high, has good resistance to persistence.
Embodiment
Be some examples described in the invention below, just to aid illustration of the present invention, if there are personnel that foregoing invention is made nonessential modification or adjusted, still belong to protection domain.
Embodiment 1.
Get 100 part 1,3-2-glycidyl-S-triazinetrione, puts into 1000mL single port flask, add 2 parts of diethylenetriamines, 1 part of carbonyl diamine, open Rotary Evaporators and heat up (oil bath heating), speed is 3 ℃/min, be warming up to 60 ℃, stop heating up, continue to stir 20 minutes, then add 0.1 part of IPDI, 0.01 part of antioxidant AT215,0.01 dibutyl tin laurate, is warming up to 130 ℃, rotary distillation 3h, obtains thick softening agent after modification.
Embodiment 2.
Get 100 part 1,3-2-glycidyl-S-triazinetrione, puts into 1000mL single port flask, add 4 parts of diethylenetriamines, 3 parts of carbonyl diamines, open Rotary Evaporators and heat up (oil bath heating), speed is 2 ℃/min, is warming up to after 70 ℃, stop heating up, continue to stir 30 minutes, then add 0.4 IPDI, 0.03 antioxidant DSTDP, 0.3 stannous octoate and tetrabutyl titanate, be warming up to 130 ℃, rotary distillation 3h, makes thick softening agent after modification.
Embodiment 3.
Get 100 part 1, 3-2-glycidyl-S-triazinetrione is put into 1000mL single port flask, add 5 parts of diethylenetriamines, 4 parts of carbonyl diamines, open Rotary Evaporators intensification (oil bath heating), speed is 2 ℃/min, be warming up to after 80 ℃, stop heating up, continue to stir 30 minutes, then add 0.9 part of IPDI, 0.07 part of antioxidant AT215 and antioxidant DSTDP(blending ratio 1:1), 0.7 part of dibutyl tin laurate and tetrabutyl titanate (both blending ratio 1:1), be warming up to 140 ℃, rotary distillation 5h, make thick softening agent after modification.
Embodiment 4.
Get 100 part 1, 3-2-glycidyl-S-triazinetrione is put into 1000mL single port flask, add 6 parts of diethylenetriamines, 5 parts of carbonyl diamines, open Rotary Evaporators intensification (oil bath heating), speed is 3 ℃/min, be warming up to after 80 ℃, stop heating up, continue to stir 30 minutes, then add 1 part of IPDI, 0.3 4 (β-(3, tri-grades of butyl-4-hydroxy phenyls of 5-) propionic acid) pentaerythritol ester and antioxidant DSTDP(mix with 1:4), 1.15 dibutyl tin laurate, stannous octoate and tetrabutyl titanate (with 1:1:1, mixing), be warming up to 140 ℃, rotary distillation 5h, make thick softening agent after modification.
Softening agent prepared by embodiment 1-4 is for PVC artificial leather product, and tensile strength index is as follows:
| Formula | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 |
| Raw material | 100 | 100 | 100 | 100 |
| Diethylenetriamine | 2 | 4 | 5 | 6 |
| Carbonyl diamine | 1 | 3 | 4 | 5 |
| IPDI | 0.1 | 0.4 | 0.9 | 1 |
| Antioxidant | 0.01 | 0.03 | 0.07 | 0.3 |
| Catalyzer | 0.01 | 0.3 | 0.7 | 1.15 |
| Tensile strength (kgf/cm 2) | 40.2 | 41.5 | 42.3 | 41.0 |
Claims (4)
1. a flexible PVC softening agent, is characterized in that being comprised of following raw materials in part by weight:
1,3-2-glycidyl-S-triazinetrione 100, diethylenetriamine 2-6, carbonyl diamine 1-5, isophorone diisocyanate 0.1-1, antioxidant 0.01-0.3, catalyzer 0.01-1.15.
2. a kind of flexible PVC softening agent according to claim 1, it is characterized in that: described antioxidant is a kind of, two or more mixture in antioxidant AT215, antioxidant DSTDP or four (β-(tri-grades of butyl-4-hydroxy phenyls of 3,5-) propionic acid) pentaerythritol ester.
3. a kind of flexible PVC softening agent according to claim 1, is characterized in that: described catalyzer is a kind of, two or more mixture in dibutyl tin laurate, stannous octoate or tetrabutyl titanate.
4. prepare the method for a kind of flexible PVC softening agent claimed in claim 1, it is characterized in that comprising the following steps:
By proportioning claimed in claim 1, by 1,3-2-glycidyl-S-triazinetrione is put into 1000mL single port flask, adds diethylenetriamine, carbonyl diamine, opens Rotary Evaporators and heats up, after being warming up to 60-80 ℃, stop heating up, continue to stir 10-30min, then add isophorone diisocyanate, antioxidant, catalyzer, be warming up to 120-140 ℃, rotary distillation 2-5h, obtains finished product.
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| CN201210175998.XA CN102675773B (en) | 2012-05-31 | 2012-05-31 | Soft poly vinyl chloride (PVC) plasticizer and preparation method thereof |
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| CN201210175998.XA CN102675773B (en) | 2012-05-31 | 2012-05-31 | Soft poly vinyl chloride (PVC) plasticizer and preparation method thereof |
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| CN102675773A CN102675773A (en) | 2012-09-19 |
| CN102675773B true CN102675773B (en) | 2014-02-12 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| RU2583812C2 (en) * | 2013-06-04 | 2016-05-10 | Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Казанский государственный архитектурно-строительный университет" КГАСУ | Polyvinyl chloride-based polymer composition |
Citations (6)
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|---|---|---|---|---|
| CN1183795A (en) * | 1995-02-16 | 1998-06-03 | 美国3M公司 | Articles incorporating pressure-sensitive adhesives having improved adhesion ot plasticized polyvinyl chloride |
| CN1294148A (en) * | 1999-11-02 | 2001-05-09 | 海尔科化工程塑料国家工程研究中心有限公司 | Non-toxic polyvinyl chloride composition and its preparing process |
| CN101331170A (en) * | 2005-11-14 | 2008-12-24 | Isp投资有限公司 | Plasticized PVC compositions |
| CN101746084A (en) * | 2008-12-05 | 2010-06-23 | 通用电气公司 | Products, laminated products and combining method thereof |
| CN101768313A (en) * | 2009-12-23 | 2010-07-07 | 宁波先锋新材料股份有限公司 | Transparent flame retarding polyvinyl chloride (PVC) composite and preparation method thereof |
| CN102227814A (en) * | 2008-11-28 | 2011-10-26 | 日产化学工业株式会社 | Composition for forming gate dielectric film of thin film transistor |
-
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- 2012-05-31 CN CN201210175998.XA patent/CN102675773B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1183795A (en) * | 1995-02-16 | 1998-06-03 | 美国3M公司 | Articles incorporating pressure-sensitive adhesives having improved adhesion ot plasticized polyvinyl chloride |
| CN1294148A (en) * | 1999-11-02 | 2001-05-09 | 海尔科化工程塑料国家工程研究中心有限公司 | Non-toxic polyvinyl chloride composition and its preparing process |
| CN101331170A (en) * | 2005-11-14 | 2008-12-24 | Isp投资有限公司 | Plasticized PVC compositions |
| CN102227814A (en) * | 2008-11-28 | 2011-10-26 | 日产化学工业株式会社 | Composition for forming gate dielectric film of thin film transistor |
| CN101746084A (en) * | 2008-12-05 | 2010-06-23 | 通用电气公司 | Products, laminated products and combining method thereof |
| CN101768313A (en) * | 2009-12-23 | 2010-07-07 | 宁波先锋新材料股份有限公司 | Transparent flame retarding polyvinyl chloride (PVC) composite and preparation method thereof |
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