CN104163960B - Magnesium oxide zinc oxide compound vulcanizing agent for neoprene sulfuration and preparation method thereof - Google Patents
Magnesium oxide zinc oxide compound vulcanizing agent for neoprene sulfuration and preparation method thereof Download PDFInfo
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- CN104163960B CN104163960B CN201410358985.5A CN201410358985A CN104163960B CN 104163960 B CN104163960 B CN 104163960B CN 201410358985 A CN201410358985 A CN 201410358985A CN 104163960 B CN104163960 B CN 104163960B
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Abstract
The present invention relates to a kind of magnesium oxide zinc oxide compound vulcanizing agent and preparation method thereof for neoprene sulfuration, this vulcanizing agent is made up of following components: activated magnesia and activated zinc oxide mixture 80.0% 90.0%；Dispersant 10.0% 20.0%；Activated magnesia and activated zinc oxide weight ratio are 1:0.2 3.0.Its preparation method is: a, activated magnesia and activated zinc oxide are mixed to get substance A, and dispersant is dissolved in dehydrated alcohol and obtains substance B；B, substance B carry out surface coating modification to substance A and obtain compound thing；C, compound thing heated and stirred is obtained ointment shape or thick magnesium oxide zinc oxide compound vulcanizing agent.This vulcanizing agent solves conventional vulcanized dose and joins in neoprene with powder, cause the problems such as the powder body uneven and MgO activity easily inefficacy of dispersion, improve the dispersibility of zinc oxide and the active retentivity of magnesium oxide, the incipient scorch simultaneously reducing high Mooney viscosity sizing material is dangerous.
Description
Technical field
The present invention relates to a kind of vulcanizing agent for neoprene sulfuration, particularly relate to a kind of magnesium oxide zinc oxide compound sulfur
Agent, meanwhile, the invention still further relates to the preparation method of a kind of magnesium oxide zinc oxide compound vulcanizing agent for neoprene sulfuration.
Background technology
Neoprene is one of elastomeric principal item, as a kind of universal specific rubber, has good resistance to
The excellent specific properties such as combustion hot, resistance to, oil resistant, resistance to chemical attack, occupy critical role in synthetic rubber.Used according to manufacturing process
The difference of molecular weight regulator, neoprene can be divided into sulfur adjustment type, non-sulfur adjustment type and mixing adjustment type, and the most non-sulfur regulates
Type is world's principal item.According to crystallization rate or the difference of degree, neoprene is divided into universal and tailored version, the most bonding
Agent special bonding type, the cold-resistant special cold resisting type of goods and oil-resisting type, cable tailored version etc..
Neoprene must sufficiently vulcanize could play heat-resisting, corrosion-resistant and ageing-resistant spy to greatest extent
Point, however in neoprene, owing to chlorine atom is in allylic positions, the most unstable, easily form hydrogen chloride, hydrogen chloride is not
Only affect curability and the physical property of sizing material, also will affect the serviceability of product, so industry is widely used with metal
Oxide is as the acceptor of chlorine atom, for the sulfuration of neoprene.
Metal current oxide shares with zinc oxide and magnesium oxide and has reasonable cure efficiency, and process safety,
Vulcanite functional.When being used alone activated zinc oxide, activated zinc oxide produces zinc chloride with hydrogen chloride fast reaction,
Add the danger of sizing material incipient scorch；Add extra light calcined magnesia while adding activated zinc oxide, activated magnesia can be made
React with zinc chloride, generate zinc oxide, so can avoid the formation of substantial amounts of zinc chloride, prevent sizing material incipient scorch, simultaneously by new life
Zinc oxide be re-used for vulcanization reaction, thus increase final neoprene crosslinking degree.But, activated zinc oxide is at neoprene
Rubber is difficult to dispersion, increases glue and burn danger；And activated magnesia the most easily makes moist and CO2Reaction so that it is activity
Reduce, the impact of sizing material coke burning performance is reduced.
Summary of the invention
For solve the deficiencies in the prior art, the invention provides a kind of be beneficial to dispersion and activity keep for chlorine
The magnesium oxide zinc oxide compound vulcanizing agent of buna sulfuration.
For achieving the above object, of the present invention for neoprene sulfuration magnesium oxide zinc oxide compound vulcanizing agent by with
Lower components by weight percent is made: activated magnesia and activated zinc oxide mixture 80.0%-90.0%；Dispersant 10.0%-20.0%；Mixing
Thing activated magnesia is 1:0.2-3.0 with the weight ratio of activated zinc oxide.
Activated magnesia constitutes the antiscorching agent in vulcanizing agent, and activated zinc oxide constitutes the activating agent in vulcanizing agent and inhales acid
Agent；Dispersant carries out Surface coating to activated magnesia and activated zinc oxide so that pulverulent mixture forms ointment shape or thickness
Shape material, improves the mixture stability in neoprene sulfidation, and meanwhile, dispersant is also to activated magnesia and activity
Zinc oxide has carried out surface modification so that in ointment or thick vulcanizing agent can be good at being dispersed in neoprene, fills
The suction acid of activated magnesia and activated zinc oxide, sulfurization are waved in distribution.
As the restriction of aforesaid way, described mixture activated magnesia is 1:1.0-with the weight ratio of activated zinc oxide
2.0。
Owing to activated magnesia is used as antiscorching agent, if activated magnesia ratio is low, the easy incipient scorch of neoprene, cause sulfuration
Degree is inadequate；Activated zinc oxide is used as activating agent and acid-acceptor, if activated magnesia ratio is high, can make again vulcanizate heat resistance
Reduce；Therefore, present invention defines more excellent ratio interval, interval vulcanizing agent prepared state of cure (vulcanization) to neoprene at this
Problem that is more excellent, that do not have incipient scorch, and heat resistance is good.
As the restriction to aforesaid way, described activated magnesia is the industrial activated light magnesium oxide of activity-80.
The Mooney scorch time of the activity influence neoprene of magnesium oxide, selects the industrial activated lightweight oxidation of activity-80
The Mooney scorch time of magnesium neoprene is the longest, when activity is more than 80, and MgO activity affects not extending Mooney scorch time
Greatly.
As the restriction to aforesaid way, described activated magnesia bulk density is 0.12-0.20g/mL.
Bulk density is big, easily occurs precipitate in magnesium oxide；Bulk density is little, and magnesium oxide is easily raised in using operating process
Dirt, causes severe operational environment, therefore bulk density is set to 0.12-0.20g/mL, makes the vulcanizing agent performance prepared more excellent.
As the restriction to aforesaid way, in described active oxidation magnesium raw material, the content of oxidation of impurities calcium is not more than 0.8%.
Impurity calcium affects the quality of neoprene, and calcium content height can make rubber layering or the phenomenon that becomes fragile occur, and calcium is main
Introduced by active oxidation magnesium raw material, therefore the content of oxidation of impurities calcium in raw materials of magnesium oxide is defined to no more than 0.8%, enters one
Step optimizes curability, improves the quality of neoprene.
As the restriction to aforesaid way, the hydrochloric acid insoluble substance content in described active oxidation magnesium raw material is not more than 0.1%.
Hydrochloric acid insoluble substance content is high, and neoprene can be caused the problems such as foaming, trachoma occur, therefore that activated magnesia is former
In material, the content of hydrochloric acid insoluble substance is defined to no more than 0.1%, optimizes curability further, improves the quality of neoprene.
As the restriction to aforesaid way, described activated zinc oxide D50 particle diameter is at 50nm-100nm；Activated magnesia D50
Particle diameter is in 0.3 μm-3 μm.
The structure composition of this vulcanizing agent is the activated zinc oxide granule first dispersed active oxidation magnesium surface that sticks to, then by
The magnesium oxide zinc oxide hybrid particles adhered to each other is carried out surface coating modification by dispersant.Due to activated zinc oxide density
Greatly, then easily precipitate when particle diameter is big, thus cause disperseing uneven；Activated magnesia particle diameter is the least, then specific surface area is the biggest, with
Neoprene active area is the biggest, is beneficial to prevent gelling phenomenon.Therefore in the preparation process of vulcanizing agent, preferably go out active oxygen
Change zinc D50 particle diameter is at 50nm-100nm, and activated magnesia D50 particle diameter is at 0.3 μm-3 μm, now activated zinc oxide and active oxygen
Change the more readily dispersible adhesion of magnesium, form the mixture of uniformly and beneficially activation plays, provide for dispersant-coated modification afterwards
Optimal structural framing, thus be beneficial to be easily dispersed and activity stabilized high performance vulcanization agent.
As the restriction to aforesaid way, described dispersant be chlorinated paraffin 52, olein, tristerin or
One or both in tripalmitin.
Dispersant, for activated magnesia and activated zinc oxide carry out surface modification, accelerates magnesium oxide and zinc oxide at chlorine
Dispersion in buna, improves dispersed homogeneous degree；Meanwhile, dispersant to activated magnesia and the Surface coating of activated zinc oxide,
Protect magnesium oxide zinc oxide in dispersive process from the impurity impact on activity so that it is play optimum in neoprene
Activity.
The preparation method that magnesium oxide zinc oxide for neoprene sulfuration of the present invention mixes vulcanizing agent mutually includes following
Step:
A, activated magnesia and activated zinc oxide are mixed, obtain substance A；By dispersant according to 1.0:1.0-1.5
Part by weight mix with dehydrated alcohol, stirring, treat that dispersant all dissolves and obtain substance B；
B, substance A is placed in high-shear emulsion machine, uniform with 2000-3000r/min Rate Dispersion, make activated zinc oxide
Stick to active oxidation magnesium surface；Substance B is uniformly sprayed at the magnesium oxide zinc oxide solid being in high-speed stirred admixture
On powder, enable dispersant to be evenly coated at solid powder surface, form coating film, disperse 10-30min, obtain magnesium oxide
Zinc oxide compound thing；
C, compound thing step b obtained are placed in thermostatic mixer, heat while stirring, and make the ethanol in solution volatilize
Going out, until system becomes ointment shape or thick magnesium oxide zinc oxide compound vulcanizing agent, wherein thermostat temperature is 40-100
℃。
Solid-liquid material is mixed by preparation process respectively, is in order to the problem preventing solid dispersion uneven occurs.Oxidation
Fully dispersed through high-shear emulsion machine of magnesium zinc oxide mix, makes adhesion uniform；The most under high velocity agitation will be dissolved with dividing
The ethanol solution of powder carries out spraying cladding, forms Modified Membrane；Finally alcohol solvent is made to wave under conditions of heating while stirring
Send out, obtain ointment shape or thick vulcanizing agent.
As the restriction to aforesaid way, the thermostat temperature of described step c is 60-80 DEG C.
The quick volatilization of ethanol in compound thing it is more conducive to, to prepare more excellent vulcanizing agent under the thermostat temperature of 60-80 DEG C.
In sum, use technical scheme, the powdery mixed system of magnesium oxide zinc oxide adds dispersion
Agent, makes ointment shape or thick magnesium oxide zinc oxide compound vulcanizing agent, solve traditional magnesium oxide zinc oxide vulcanizing agent with
Powder joins in neoprene, easily cause the powder body uneven and activated magnesia of dispersion be vulnerable to moisture in air and
CO2Impact and the problems such as inefficacy, improve the dispersibility of activated zinc oxide and the active retentivity of activated magnesia；Drop simultaneously
The incipient scorch of low high Mooney viscosity sizing material is dangerous, provides one for the sulfuration of neoprene and is easy to application, and curing efficiency is more
High magnesium oxide zinc oxide compound vulcanizing agent.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is further illustrated.
Embodiment one
The present embodiment relates to the preparation method of a kind of magnesium oxide zinc oxide compound vulcanizing agent for neoprene sulfuration, should
Method comprises the following steps:
A, take activated zinc oxide and mix with activated magnesia, be designated as substance A；Dispersant is poured into and fills 30ml dehydrated alcohol
Solution stirs, after being completely dissolved, is designated as substance B；
B, substance A is placed in high-shear emulsion machine, uniform with 2000-3000r/min Rate Dispersion, make zinc oxide adhere to
At mgo surface；Substance B is uniformly sprayed in the magnesium oxide zinc oxide solid powder being in high-speed stirred admixture, makes
Dispersant can be evenly coated at solid powder surface, forms coating film, disperses 10-30min, obtains magnesium oxide and zinc oxide is multiple
Mixed thing；
C, compound system step b obtained are placed in thermostatic mixer, heat while stirring, and make the ethanol in solution wave
Sending out, until system becomes ointment shape or thick, i.e. obtain magnesium oxide zinc oxide compound vulcanizing agent, wherein thermostat temperature is
40-100℃。
Embodiment two
Following embodiment relate to the magnesium oxide zinc oxide compound vulcanizing agent for neoprene sulfuration, and it all uses reality
Executing the preparation method of example one, difference is the consumption of each raw material composition, as shown in the table:
Compound vulcanizing agent various embodiments above obtained is used for vulcanizing neoprene, carries out the neoprene after sulfuration
Performance evaluation.Measure Mooney scorch time by mooney's viscosimeter, test hot strength, result according to GB GB/T528-1998
As shown in the table.
With the high-class product of conventional powder vulcanizing agent, neoprene is vulcanized, during its mooney scorch of the neoprene obtained
Between be 30-60MSt5/ min, hot strength is >=24.0MPa.Each embodiment result shown in upper table is vulcanized with conventional powder
The neoprene performance of agent high-class product sulfuration contrasts, and result shows, the magnesium oxide zinc oxide compound sulfuration that the present invention prepares
Agent can make the neoprene Mooney scorch time after sulfuration longer, and hot strength is higher.
Claims (9)
1. the magnesium oxide zinc oxide compound vulcanizing agent for neoprene sulfuration, it is characterised in that this vulcanizing agent is by following
Components by weight percent is made: activated magnesia and activated zinc oxide mixture 80.0%-90.0%；Dispersant 10.0%-20.0%；Mixture
Activated magnesia is 1:0.2-3.0 with the weight ratio of activated zinc oxide；
Preparation method comprises the following steps:
A, activated magnesia and activated zinc oxide are mixed, obtain substance A；By dispersant according to the weight of 1.0:1.0-1.5
Amount ratio mixes with dehydrated alcohol, stirring, treats that dispersant all dissolves and obtains substance B；
B, substance A is placed in high-shear emulsion machine, uniform with 2000-3000r/min Rate Dispersion, make activated zinc oxide adhere to
At active oxidation magnesium surface；Substance B is uniformly sprayed at the magnesium oxide zinc oxide solid powder being in high-speed stirred admixture
On, enable dispersant to be evenly coated at solid powder surface, form coating film, disperse 10-30min, obtain magnesium oxide oxidation
Zinc compound thing；
C, compound thing step b obtained are placed in thermostatic mixer, heat while stirring, and make the ethanol in solution volatilize
Going, until system becomes ointment shape or thick magnesium oxide zinc oxide compound vulcanizing agent, wherein thermostat temperature is 40-100 DEG C.
2., according to the magnesium oxide zinc oxide compound vulcanizing agent for neoprene sulfuration described in claim 1, its feature exists
In: described mixture activated magnesia is 1:1.0-2.0 with the weight ratio of activated zinc oxide.
3., according to the magnesium oxide zinc oxide compound vulcanizing agent for neoprene sulfuration described in claim 1, its feature exists
In: described activated magnesia is the industrial activated light magnesium oxide of activity-80.
4., according to the magnesium oxide zinc oxide compound vulcanizing agent for neoprene sulfuration described in claim 1, its feature exists
In: described activated magnesia bulk density is 0.12-0.20g/mL.
5., according to the magnesium oxide zinc oxide compound vulcanizing agent for neoprene sulfuration described in claim 1, its feature exists
In: in described active oxidation magnesium raw material, the content of oxidation of impurities calcium is not more than 0.8%.
6., according to the magnesium oxide zinc oxide compound vulcanizing agent for neoprene sulfuration described in claim 1, its feature exists
In: the hydrochloric acid insoluble substance content in described active oxidation magnesium raw material is not more than 0.1%.
7., according to the magnesium oxide zinc oxide compound vulcanizing agent for neoprene sulfuration described in claim 1, its feature exists
In: described activated zinc oxide D50 particle diameter is at 50nm-100nm；Activated magnesia D50 particle diameter is in 0.3 μm-3 μm.
8., according to the magnesium oxide zinc oxide compound vulcanizing agent for neoprene sulfuration described in claim 1, its feature exists
In: dispersant is one or both in chlorinated paraffin 52, olein, tristerin or tripalmitin.
9., according to the magnesium oxide zinc oxide compound vulcanizing agent for neoprene sulfuration described in claim 1, its feature exists
In: the preferred thermostat temperature of described step c is 60-80 DEG C.
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| CN201410358985.5A CN104163960B (en) | 2014-07-24 | 2014-07-24 | Magnesium oxide zinc oxide compound vulcanizing agent for neoprene sulfuration and preparation method thereof |
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| CN107082923B (en) * | 2017-05-22 | 2019-03-05 | 河北镁神科技股份有限公司 | A kind of calcium and magnesium zinc composite powder material and preparation method thereof for neoprene vulcanization reinforcement |
| CN113755031A (en) * | 2021-10-22 | 2021-12-07 | 安徽锦华氧化锌有限公司 | Dispersing and activating treatment method for zinc oxide |
| CN115386141B (en) * | 2022-09-02 | 2023-09-01 | 常州市五洲环保科技有限公司 | Organic zinc rubber processing aid and preparation method thereof |
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| CN101787149A (en) * | 2010-01-29 | 2010-07-28 | 铁岭华晨橡塑制品有限公司 | Sizing formula of flame-retarding elastic support rubber product |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101787149A (en) * | 2010-01-29 | 2010-07-28 | 铁岭华晨橡塑制品有限公司 | Sizing formula of flame-retarding elastic support rubber product |
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Address after: No. 26 Yuxiang street, Shijiazhuang, Hebei Province, Hebei Co-patentee after: HEBEI MEISHEN TECHNOLOGY CO.,LTD. Patentee after: HEBEI University OF SCIENCE AND TECHNOLOGY Address before: No. 26 Yuxiang street, Shijiazhuang, Hebei Province, Hebei Co-patentee before: HEBEI MEISHEN TECHNOLOGY CO.,LTD. Patentee before: Hebei University of Science and Technology |
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