CN106118743A - A kind of environmentally friendly preparation method of chlorinated paraffin - Google Patents

A kind of environmentally friendly preparation method of chlorinated paraffin Download PDF

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Publication number
CN106118743A
CN106118743A CN201610627194.7A CN201610627194A CN106118743A CN 106118743 A CN106118743 A CN 106118743A CN 201610627194 A CN201610627194 A CN 201610627194A CN 106118743 A CN106118743 A CN 106118743A
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CN
China
Prior art keywords
chlorinated paraffin
stabilizer
chlorine
environmentally friendly
paraffin
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Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
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CN201610627194.7A
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Chinese (zh)
Inventor
苏振生
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Anhui China Mstar Technology Ltd
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Anhui China Mstar Technology Ltd
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Priority to CN201610627194.7A priority Critical patent/CN106118743A/en
Publication of CN106118743A publication Critical patent/CN106118743A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10GCRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G73/00Recovery or refining of mineral waxes, e.g. montan wax
    • C10G73/38Chemical modification of petroleum
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10GCRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G2300/00Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
    • C10G2300/10Feedstock materials

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  • Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention discloses the environmentally friendly preparation method of a kind of chlorinated paraffin: (1). liquid paraffin raw material is joined in chlorination reactor, is heated to 30 DEG C 60 DEG C, add the catalyst of liquid paraffin weight 0.1 10%;(2). radiating with 40 60W electric filament lamp, be slowly introducing chlorine simultaneously in reactor, control reaction temperature, in the range of 90 DEG C 100 DEG C, reacts 90 110min, when reaction mass density reaches about 1.25 grams/cc, stops logical chlorine;(3) it is passed through nitrogen, drives the hydrogen chloride and unreacted a small amount of chlorine generated in course of reaction out of, in material, add weight of material 0.05~the stabilizer of 0.15%, stir, cool down and i.e. obtain chlorinated paraffin 52.The preparation method of the chlorinated paraffin that the present invention provides, technique is simple, and the response time is short, and chlorine consumption is few, conversion ratio is high, reduces production cost, and liquid paraffin raw material is not required to refine, without spent acid, waste sludge discharge, environmental protection, there is preferable economic benefit and social benefit.

Description

A kind of environmentally friendly preparation method of chlorinated paraffin
Technical field
The present invention relates to the preparation method of a kind of fire retardant, be specifically related to the environmentally friendly preparation side of a kind of chlorinated paraffin Method.
Background technology
Chlorinated paraffin has that volatility is low, fire-retardant, electrical insulating property is good and many excellent physicochemical properties such as resistance to chemical attack, Can be used as fire retardant polrvinyl chloride secondary plasticizer(-iser) etc., be widely used in produce plastics, cable, plate, flexible pipe, artificial leather and Rubbers etc. are it can also be used to the additive of paint, coating and lubricating oil etc..Due to important in commercial Application of chlorinated paraffin Property, the therefore optimization of its production method, arouse widespread concern.
At present, the mode of production of chlorinated paraffin mainly has thermal chlorination and photocatalytic method.
The thermal chlorination response time is long, and the response time such as chlorinated paraffin-52 is typically for up to about 60h, causes production efficiency The phenomenon such as low, energy consumption is high and chlorine utilization is low highlights.
Photocatalytic method is to promote chlorine molecule covalent bond fission to be dissociated into chlorine radical with the ultraviolet light of about 340nm, activation The chlorine radical of state bombards paraffin molecule continuously and forms C-Cl key, accelerates reaction rate, generates the response time of paraffin-52 It is down to 24-36h (and 24-38h.But, the theoretical and practical production experience according to bimodulus, the course of reaction of chlorinated paraffin is homogeneous Reaction, chlorine is first dissolved in paraffin the most just chemical reaction, and chlorine dissolution velocity in paraffin is less than response speed, The most whole reaction is mass transport limitation step
In three of the above mode, it is the most extensive that the mode of the third employing light chlorination process is applied, in order to use continuously Property and producing on a large scale, can use multiple reactor in prior art is used in series, such as Patent No. 200610025410.7 In the Chinese patent of entitled " method of continuous prodution chlorinated paraffin ", just used this mode, then regardless of In the method for the consecutive production chlorinated paraffin of mode, each reactor all can produce tail gas, and tail gas is chlorine and chlorination Hydrogen, in existing method, is directly to be collected by the tail gas produced in each reactor, enters in exhaust treatment system, This mode, becomes huge by the supply making chlorine, the most well utilizes for chlorine present in tail gas, increases Add production cost.
Summary of the invention
It is an object of the invention to, it is provided that the preparation method of a kind of chlorinated paraffin, technique is simple, and the response time is short, chlorine Consuming few, conversion ratio is high, reduces production cost.
Technical scheme is as follows:
A kind of environmentally friendly preparation method of chlorinated paraffin, it comprises the following steps:
(1). liquid paraffin raw material is joined in chlorination reactor, is heated to 30 DEG C-60 DEG C, add liquid paraffin weight The catalyst of 0.1-10%;
(2). radiate with 40-60W electric filament lamp, in reactor, be slowly introducing chlorine simultaneously, control reaction temperature and exist In the range of 90 DEG C-100 DEG C, react 90-110min, when reaction mass density reaches about 1.25 grams/cc, stop logical chlorine Gas;
(3) it is passed through nitrogen, drives the hydrogen chloride and unreacted a small amount of chlorine generated in course of reaction out of, add in material Weight of material 0.05~the stabilizer of 0.15%, stir, and cools down and i.e. obtains chlorinated paraffin-52.
Stabilizer is heat stabilizer and light stabilizer.
Heat stabilizer be the one in Ethylene glycol diglycidyl ether, HFW 2 complex stabilizer, epoxy soybean oil or Several.
Light stabilizer is ESCALOL 567.
The preparation method of chlorinated paraffin that the present invention provides, it has the beneficial effects that, technique is simple, and the response time is short, chlorine Gas consumption is few, and conversion ratio is high, reduces production cost, and liquid paraffin raw material is not required to refine, without spent acid, waste sludge discharge, and green ring Protect, there is preferable economic benefit and social benefit.
Detailed description of the invention
Below in conjunction with specific embodiment the present invention made and further illustrating.
Embodiment 1
A kind of environmentally friendly preparation method of chlorinated paraffin, it comprises the following steps:
(1). liquid paraffin raw material is joined in chlorination reactor, is heated to 60 DEG C, add liquid paraffin weight 1% Catalyst;
(2). radiate with 60W electric filament lamp, in reactor, be slowly introducing chlorine simultaneously, control reaction temperature 100 In the range of DEG C, react 110min, when reaction mass density reaches about 1.25 grams/cc, stop logical chlorine;
(3) it is passed through nitrogen, drives the hydrogen chloride and unreacted a small amount of chlorine generated in course of reaction out of, add in material The stabilizer of weight of material 0.15%, stirs, and cools down and i.e. obtains chlorinated paraffin-52.
Stabilizer is heat stabilizer and light stabilizer.
Heat stabilizer is HFW 2 complex stabilizer.
Embodiment 2
A kind of environmentally friendly preparation method of chlorinated paraffin, it comprises the following steps:
(1). liquid paraffin raw material is joined in chlorination reactor, is heated to 30 DEG C, add liquid paraffin weight 0.1 Catalyst;
(2). radiate with 40W electric filament lamp, in reactor, be slowly introducing chlorine simultaneously, control reaction temperature at 90 DEG C In the range of, react 110min, when reaction mass density reaches about 1.25 grams/cc, stop logical chlorine;
(3) it is passed through nitrogen, drives the hydrogen chloride and unreacted a small amount of chlorine generated in course of reaction out of, add in material The stabilizer of weight of material 0.05%, stirs, and cools down and i.e. obtains chlorinated paraffin-52.
Stabilizer is heat stabilizer and light stabilizer.
Heat stabilizer is Ethylene glycol diglycidyl ether.
Embodiment 3
A kind of environmentally friendly preparation method of chlorinated paraffin, it comprises the following steps:
(1). liquid paraffin raw material is joined in chlorination reactor, is heated to 50 DEG C, add liquid paraffin weight 2% Catalyst;
(2). radiate with 50W electric filament lamp, in reactor, be slowly introducing chlorine simultaneously, control reaction temperature at 95 DEG C In the range of, react 100min, when reaction mass density reaches about 1.25 grams/cc, stop logical chlorine;
(3) it is passed through nitrogen, drives the hydrogen chloride and unreacted a small amount of chlorine generated in course of reaction out of, add in material The stabilizer of weight of material 0.1, stirs, and cools down and i.e. obtains chlorinated paraffin-52.
Stabilizer is heat stabilizer and light stabilizer.
Heat stabilizer is in epoxy soybean oil.
Light stabilizer is ESCALOL 567.

Claims (4)

1. the environmentally friendly preparation method of a chlorinated paraffin, it is characterised in that: it comprises the following steps:
(1). liquid paraffin raw material is joined in chlorination reactor, is heated to 30 DEG C-60 DEG C, add liquid paraffin weight 0.1- The catalyst of 10%;
(2). radiate with 40-60W electric filament lamp, in reactor, be slowly introducing chlorine simultaneously, control reaction temperature 90 DEG C- In the range of 100 DEG C, react 90-110min, when reaction mass density reaches about 1.25 grams/cc, stop logical chlorine;
(3) it is passed through nitrogen, drives the hydrogen chloride and unreacted a small amount of chlorine generated in course of reaction out of, in material, add material Weight 0.05~the stabilizer of 0.15%, stir, and cools down and i.e. obtains chlorinated paraffin-52.
The environmentally friendly preparation method of chlorinated paraffin the most according to claim 1, it is characterised in that: described stabilizer is Heat stabilizer and light stabilizer.
The environmentally friendly preparation method of chlorinated paraffin the most according to claim 2, it is characterised in that: described heat stabilizer For one or several in Ethylene glycol diglycidyl ether, HFW 2 complex stabilizer, epoxy soybean oil.
The environmentally friendly preparation method of chlorinated paraffin the most according to claim 2, it is characterised in that: described light stabilizer For ESCALOL 567.
CN201610627194.7A 2016-08-03 2016-08-03 A kind of environmentally friendly preparation method of chlorinated paraffin Pending CN106118743A (en)

Priority Applications (1)

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Application Number Priority Date Filing Date Title
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CN106118743A true CN106118743A (en) 2016-11-16

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107142124A (en) * 2017-06-26 2017-09-08 柳州市隆达丰化工科技有限公司 A kind of method that thermal chlorination is combined production chlorinated paraffin 52 with photocatalytic method
CN107245350A (en) * 2017-06-26 2017-10-13 柳州市隆达丰化工科技有限公司 A kind of method that thermal chlorination is combined production chlorinated paraffin 70 with photocatalytic method
CN111592913A (en) * 2020-05-21 2020-08-28 广州鑫泓设备设计有限公司 Chlorinated paraffin production process capable of improving utilization rate of raw material resources
CN112011367A (en) * 2019-05-31 2020-12-01 江苏国威化工有限公司 Chlorinated paraffin for rubber and plastic foaming and preparation method thereof
CN116179009A (en) * 2022-12-28 2023-05-30 北京东方雨虹防水技术股份有限公司 Paraffin oil modifier and preparation method thereof, waterproof coating containing paraffin oil modifier and preparation method of waterproof coating

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103849433A (en) * 2013-03-26 2014-06-11 洛阳欧克迈自控工程有限公司 Automatic production technology of chlorinated paraffin
CN104593071A (en) * 2013-10-30 2015-05-06 青岛旺裕橡胶制品有限公司 Preparation method of chlorinated paraffin

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103849433A (en) * 2013-03-26 2014-06-11 洛阳欧克迈自控工程有限公司 Automatic production technology of chlorinated paraffin
CN104593071A (en) * 2013-10-30 2015-05-06 青岛旺裕橡胶制品有限公司 Preparation method of chlorinated paraffin

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
刘发起: ""催化氯化法合成氯化石蜡-52的研究"", 《精细石油化工进展》 *
郭爱花等: ""新型高效有机热稳定剂"", 《化工学报》 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107142124A (en) * 2017-06-26 2017-09-08 柳州市隆达丰化工科技有限公司 A kind of method that thermal chlorination is combined production chlorinated paraffin 52 with photocatalytic method
CN107245350A (en) * 2017-06-26 2017-10-13 柳州市隆达丰化工科技有限公司 A kind of method that thermal chlorination is combined production chlorinated paraffin 70 with photocatalytic method
CN112011367A (en) * 2019-05-31 2020-12-01 江苏国威化工有限公司 Chlorinated paraffin for rubber and plastic foaming and preparation method thereof
CN111592913A (en) * 2020-05-21 2020-08-28 广州鑫泓设备设计有限公司 Chlorinated paraffin production process capable of improving utilization rate of raw material resources
CN116179009A (en) * 2022-12-28 2023-05-30 北京东方雨虹防水技术股份有限公司 Paraffin oil modifier and preparation method thereof, waterproof coating containing paraffin oil modifier and preparation method of waterproof coating

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