CN101921348B - Method for preparing epoxidized liquid natural rubber - Google Patents
Method for preparing epoxidized liquid natural rubber Download PDFInfo
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- CN101921348B CN101921348B CN201010219750XA CN201010219750A CN101921348B CN 101921348 B CN101921348 B CN 101921348B CN 201010219750X A CN201010219750X A CN 201010219750XA CN 201010219750 A CN201010219750 A CN 201010219750A CN 101921348 B CN101921348 B CN 101921348B
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- natural rubber
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- epoxidized liquid
- epoxidized
- latex
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Abstract
The invention discloses a method for preparing epoxidized liquid natural rubber, which is characterized by adding a strong oxidizer (periodic acid) to epoxidized natural rubber at 30 DEG C to prepare the epoxidized liquid natural rubber by chemical degradation. The prepared epoxidized liquid natural rubber is a brilliant yellow liquid which is sticky and has liquidity. The new method for preparing the epoxidized liquid natural rubber has the advantages of simple technical process, less energy consumption, less pollution, short reaction time, low reaction temperature, obvious degradation effect, wide application and high economic benefit.
Description
Technical field
The present invention is the method for preparing epoxidized liquid natural rubber.Be specifically related to use a kind of strong oxidizer Periodic acid 99 H
5IO
6The chemical degradation epoxy natural rubber prepares the preparation method of epoxidized liquid natural rubber.
Background technology
Liquid natural rubber is a tree elastomer in another new variety in latest developments stage, can be applied to technical fields such as processing aid, reactive plasticizer, tackiness agent.So far, have 3 kinds to prepare the liquid natural rubber method, these methods are: oxidation reduction process, photocatalytic method, HTHP oxidation style.Traditional mode of production is employed in the method that adds peptizer on the open mixing roll of high temperature, make the number average relative molecular mass and be 39000 liquid natural rubber, but this method needs high temperature degradation, and it is bigger to consume energy, and cost is higher; Adopt photocatalytic method in addition, the liquid natural rubber performance for preparing is not fine, and structure is quite complicated, and long reaction time can not better controlled NR degradation rate, is not suitable for suitability for industrialized production.What employing was maximum at present is exactly that oxidation reduction process prepares liquid natural rubber, utilizes organic alkali catalyst such as phenylhydrazine, pyridine etc., and the degraded natural rubber latex, degradation effect is fine.In the U.S., Malaysia adopts phenylhydrazine/atmospheric oxidation reduction system to produce the liquid natural rubber technology in the latex stage, suitability for industrialized production, but phenylhydrazine has severe toxicity, can not be applied to suitability for industrialized production in China, and bigger to environmental hazard.
Epoxy natural rubber has good oil-proofness, the sliding property of good resistance to air loss, binding property and moisture-proof, and these premium propertiess are used widely epoxy natural rubber.Mainly be employed at present and with Peracetic Acid or peroxyformic acid NR carried out epoxidation under the acidic conditions and prepare ENR.
Summary of the invention
The objective of the invention is through using a kind of strong oxidizer chemical degradation epoxy natural rubber to prepare the preparation method of epoxidized liquid natural rubber.This method characteristics are: the epoxidized liquid natural rubber after the degraded is the lower molecular weight tree elastomer, has functionalization group epoxide group again, and this makes epoxidized liquid natural rubber have widely and uses.
The technical scheme that the present invention adopted is:
The epoxidized liquid natural rubber preparation method is following:
Step 1: the preparation of epoxy natural rubber latex
Utilize known method to prepare epoxy natural rubber latex.Being about to centrifugal concentrated natural latex, to be diluted to drc be 20%; Add nonionogenic tenside; Ethomeen 18/60 commonly used, make its consumption for to dried glue heavy 3%, be that 35% Peracetic Acid or peroxyformic acid solution slowly add in stable diluted latex with concentration again; The control reaction conditions is 60 ℃ * 24h, makes epoxy natural rubber latex.
Step 2: the preparation of epoxidized liquid natural rubber
Drc is the Periodic acid 99 H5IO6 that adds 0.5 mass parts in 20%～50% the epoxy natural rubber latex; The unitary mol ratio of Periodic acid 99 and epoxy is 0.24,0.51 and 1.13; React 2～21h down at 30 ℃; In methyl alcohol, precipitate then, vacuum-drying under the room temperature makes the glassy yellow epoxidized liquid natural rubber.The present invention compared with prior art has following advantage:
(1) epoxidized liquid natural rubber of this law preparation at room temperature has good flowability, and epoxy-functional is arranged, and application prospect is widely arranged.
(2) this law prepares epoxidized liquid natural rubber, and the reaction times is short, and temperature of reaction is low, and degradation effect is obvious.
(3) liquid natural rubber of this law preparation, technology is simple, and power consumption is few, and cost is low, pollutes and lacks, and is fit to suitability for industrialized production.
Embodiment
The contriver once did many successful experiments, selected following embodiment that invention further is detailed at present:
Embodiment 1:
Step 1: the preparation of epoxy natural rubber latex
Utilize known method to prepare epoxy natural rubber latex.Being about to centrifugal concentrated natural latex, to be diluted to drc be 20%; Add nonionogenic tenside; Ethomeen 18/60 commonly used, make its consumption for to dried glue heavy 3%, be that 35% Peracetic Acid or peroxyformic acid solution slowly add in stable diluted latex with concentration again; The control reaction conditions is 60 ℃ * 24h, makes epoxy natural rubber latex.
Step 2: the preparation of epoxidized liquid natural rubber
At drc is the Periodic acid 99 that adds 0.5 mass parts in 20% the epoxy natural rubber latex, and Periodic acid 99 is 0.51mol.mo than last epoxidation unit
-1, react 2h down at 30 ℃, in methyl alcohol, precipitate then, vacuum-drying under the room temperature makes the glassy yellow epoxidized liquid natural rubber, and number-average molecular weight is 11000.
Embodiment 2:
Step 1: the preparation of epoxy natural rubber latex
Utilize known method to prepare epoxy natural rubber latex.Being about to centrifugal concentrated natural latex, to be diluted to drc be 20%; Add nonionogenic tenside; Ethomeen 18/60 commonly used, make its consumption for to dried glue heavy 3%, be that 35% Peracetic Acid or peroxyformic acid solution slowly add in stable diluted latex with concentration again; The control reaction conditions is 60 ℃ * 24h, makes epoxy natural rubber latex.
Step 2: the preparation of epoxidized liquid natural rubber
At drc is the Periodic acid 99 that adds 0.5 mass parts in 35% the epoxy natural rubber latex, and Periodic acid 99 is 1.13mol.mol than last epoxidation unit
-1, react 12h down at 30 ℃, in methyl alcohol, precipitate then, vacuum-drying under the room temperature makes the glassy yellow epoxidized liquid natural rubber, and number-average molecular weight is 7200.
Embodiment 3:
Step 1: the preparation of epoxy natural rubber latex
Utilize known method to prepare epoxy natural rubber latex.Being about to centrifugal concentrated natural latex, to be diluted to drc be 20%; Add nonionogenic tenside; Ethomeen 18/60 commonly used, make its consumption for to dried glue heavy 3%, be that 35% Peracetic Acid or peroxyformic acid solution slowly add in stable diluted latex with concentration again; The control reaction conditions is 60 ℃ * 24h, makes epoxy natural rubber latex.
Step 2: the preparation of epoxidized liquid natural rubber
At drc is the Periodic acid 99 that adds 0.5 mass parts in 50% the epoxy natural rubber latex, and Periodic acid 99 is 0.24mol.mol than last epoxidation unit
-1, react 21h down at 30 ℃, in methyl alcohol, precipitate then, vacuum-drying under the room temperature makes the glassy yellow epoxidized liquid natural rubber, and number-average molecular weight is 9000.
Claims (1)
1. method for preparing epoxidized liquid natural rubber is characterized in that:
At drc is the Periodic acid 99 that adds 0.5 mass parts in 20%～50% epoxy natural rubber latex; Periodic acid 99 and epoxidation unit mol ratio are 0.24,0.51 or 1.13; React 2～21h down at 30 ℃; In methyl alcohol, precipitate then, vacuum-drying under the room temperature makes the glassy yellow epoxidized liquid natural rubber.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201010219750XA CN101921348B (en) | 2010-06-23 | 2010-06-23 | Method for preparing epoxidized liquid natural rubber |
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|---|---|---|---|
| CN201010219750XA CN101921348B (en) | 2010-06-23 | 2010-06-23 | Method for preparing epoxidized liquid natural rubber |
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| CN101921348A CN101921348A (en) | 2010-12-22 |
| CN101921348B true CN101921348B (en) | 2012-01-11 |
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| CN201010219750XA Active CN101921348B (en) | 2010-06-23 | 2010-06-23 | Method for preparing epoxidized liquid natural rubber |
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| CN109494373B (en) * | 2018-10-30 | 2021-02-19 | 桑德新能源技术开发有限公司 | Adhesive, preparation method thereof, positive electrode and lithium-sulfur battery |
| CN110183552B (en) * | 2019-04-30 | 2021-09-21 | 沈阳化工大学 | Preparation method of liquid gutta-percha |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| GB0708464D0 (en) * | 2007-05-02 | 2007-06-06 | Tun Abdul Razak Res Ct | Treatment of epoxidized natural rubber latex |
| CN101654488A (en) * | 2009-09-10 | 2010-02-24 | 中国热带农业科学院农产品加工研究所 | Technique for preparing epoxy natural rubber |
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