CN109232911A - Neoprene emulsifier and preparation method thereof - Google Patents
Neoprene emulsifier and preparation method thereof Download PDFInfo
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- CN109232911A CN109232911A CN201811172845.3A CN201811172845A CN109232911A CN 109232911 A CN109232911 A CN 109232911A CN 201811172845 A CN201811172845 A CN 201811172845A CN 109232911 A CN109232911 A CN 109232911A
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2311/00—Characterised by the use of homopolymers or copolymers of chloroprene
- C08J2311/02—Latex
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Abstract
The present invention relates to a kind of neoprene emulsifiers and preparation method thereof, and the raw material components of neoprene emulsifier are by weight, comprising: 14~20 parts by weight of 2~6 parts by weight of rosin raw material, hydroxide and/or 1 parts by weight of hydroxide aqueous solution and deionized water；Wherein, rosin raw material is rosin and/or disproportionated rosin；Hydroxide is potassium hydroxide；Hydroxide aqueous solution is sodium hydroxide solution.The present invention as raw material components and passes through scientific matching using substances such as rosin and/or disproportionated rosins, and emulsifying effectiveness can be improved in the neoprene emulsifier being prepared, so as to improve physical mechanical properties such as the breaking strength of neoprene and elasticity；And preparation method is simple, and production cost is low.
Description
Technical field
The present invention relates to chemical technology fields, and in particular to a kind of neoprene emulsifier and preparation method thereof.
Background technique
It is primary raw material progress α-polymerization and the conjunction produced that neoprene also known as chloroprene rubber, which are by chlorobutadiene,
At rubber, it is widely used in weathering resistance product, viscose glue sole, coating and rocket fuel.Neoprene is with emulsion polymerization
Production, the technological process of production is mostly one-pot batchwise polymerization.Polymerization temperature is controlled at 40~60 DEG C more, and conversion ratio is then on 90% left side
It is right.Polymerization temperature, final conversion ratio be excessively high or polymerization process in enter air (oxygen) and will lead to product quality decline.Neoprene
Rubber is different from general synthetic rubber, it does not have to sulfur cross-linking, but is vulcanized with zinc oxide, magnesia etc..In order to enhance emulsification
Effect needs that emulsifier is added in the production process of neoprene；But existing emulsifier effect is not highly desirable,
Therefore, how to prepare novel neoprene emulsifier is the direction for being worth research.
Summary of the invention
For the defects in the prior art, it is an object of that present invention to provide a kind of neoprene emulsifier and its preparation sides
Method, emulsifying effectiveness can be improved using neoprene emulsifier, so as to improve objects such as the breaking strength of neoprene and elasticity
Manage mechanical performance；And preparation method is simple, and production cost is low.
To achieve the above object, technical solution provided by the invention are as follows:
The present invention provides a kind of neoprene emulsifiers, and raw material components are by weight, comprising: 2~6 weight of rosin raw material
Measure part, 14~20 parts by weight of hydroxide and/or 1 parts by weight of hydroxide aqueous solution and deionized water.
Preferably, rosin raw material is rosin and/or disproportionated rosin.
Preferably, hydroxide is potassium hydroxide；Hydroxide aqueous solution is sodium hydroxide solution；Preferably, hydroxide
The mass concentration of sodium solution is 30%~34%.
Preferably, the raw material components of neoprene emulsifier are by weight, comprising: 5.48 parts by weight of disproportionated rosin, hydrogen
18.71 parts by weight of 1 parts by weight of potassium oxide and deionized water.
Preferably, the raw material components of neoprene emulsifier are by weight, comprising: 2.47 parts by weight of rosin, hydroxide
14.65 parts by weight of 1 parts by weight of sodium solution and deionized water；Wherein, the mass concentration of sodium hydroxide solution is 32%.
Preferably, the preparation method of rosin raw material is comprising steps of masson pine rosin, composite antioxidant and solvent are mixed equal
It is even, it then dissolves by heating, obtains mixed solution；Mixed solution is added in distilling apparatus, adjustment vacuum degree to 0.09~
0.1MPa is then heated to 200~205 DEG C, after keeping the temperature 35~40min, closes vacuum, is filled with inert gas into distilling apparatus
Pressure be zero；Vacuum is opened, adjusting vacuum degree in distilling apparatus is 80~120Pa, then heats to 219~220 DEG C, heat preservation
45~48min is distilled, vacuum is closed, being filled with pressure of the inert gas into distilling apparatus is zero, and collection evaporates excess, obtains rosin
Raw material.
It is further preferred that composite antioxidant includes antioxidant MB and antioxidant DNP；Antioxidant MB's and antioxidant DNP
Mass ratio is 1:(0.2~0.3)；Solvent is pinane.
It is further preferred that the mass ratio of masson pine rosin, composite antioxidant and solvent is 1:(0.4~0.5): (0.02
~0.03)；The heating rate used during being heated to 200~205 DEG C is 0.5~0.6 DEG C/min；It is warming up to 219~220 DEG C
The heating rate used in the process is 0.01~0.02 DEG C/min.
The present invention also provides the preparation methods of neoprene emulsifier, comprising steps of carrying out to preparing tank injection nitrogen
Nitrogen envelope, is then injected into deionized water, opens exhaust-valve, and hydroxide and/or hydroxide water is added in turn on agitator according to the ratio
Solution；Alkali content is measured by sampling after 4~6min of stirring, opens steam valve after detection is qualified and heats up；It will by electric block
Rosin raw material is proportionally added into preparing tank, closes exhaust-valve after adding material；Timing is kept the temperature after temperature rises to 92 DEG C, and is matched
Tank injection nitrogen processed carries out nitrogen envelope, adjusts steam input according to temperature, maintains 92 ± 1 DEG C always, keeps the temperature 5 hours；Wherein, timing
Sample detection solid content after heat preservation 2 hours stops stirring, the 5th hour the second solid content of sample detection when by 4 hours；Detection is closed
After lattice, cooling water circulating pump is opened, opens recirculated cooling water cooling, holding vessel preservation is pumped to when being down to 50 DEG C.It needs to illustrate
, when there is new prepared rosin soap (neoprene emulsifier) to squeeze into, holding vessel circulating pump is opened, material is carried out
Homogenizing guarantees rosin soap uniform quality；Product is pumped into tank car according to user's dosage, and user's use is sent after weighing.
Preferably, when hydroxide is potassium hydroxide, control adding rate is 19.5~20.5kg/ when adding potassium hydroxide
Min, preferably 20kg/min；Alkali content is 4.5%~5.0%, and pH value is 10~11；When hydroxide is potassium hydroxide, the
The corresponding potash soap solid content of two solid contents is 25 ± 0.5%；When hydroxide aqueous solution is sodium hydroxide solution, the second solid content
Corresponding soda soap solid content is 15 ± 0.5%.
Technical solution provided by the invention, with following the utility model has the advantages that (1) neoprene emulsifier provided by the invention
Using rosin and/or disproportionated rosin as raw material components, effect is good and environmentally friendly, is better than now to the emulsifying effectiveness of neoprene
Emulsifier；And preparation method is simple, and production cost is low；(2) it is prepared into using neoprene emulsifier provided by the invention
The modified chloroprene rubber arrived, hardness with higher, breaking strength, elasticity are more preferable, and brittle temperature reduces, physical mechanical property
It is good, there is high rigidity and high cold resistance.
Additional aspect and advantage of the invention will be set forth in part in the description, and will partially become from the following description
Obviously, or practice through the invention is recognized.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical solution of the present invention is clearly and completely described.Implement below
Example is only used for clearly illustrating technical solution of the present invention, therefore is intended only as example, and cannot be used as a limitation and limit this hair
Bright protection scope.
Experimental method in following embodiments is unless otherwise specified conventional method.Examination as used in the following examples
Material is tested, is to be commercially available from regular shops unless otherwise specified.Quantitative test in following embodiment, is respectively provided with three
Secondary to repeat to test, data are the average value or mean+SD of three repeated experiments.
The each raw material component for preparing neoprene emulsifier of the present invention can be pressed as matching in production according to parts by weight
Increase according to corresponding ratio or reduce, as large-scale production can by kilogram or as unit of ton, small-scale production can also be gram to be
Unit, weight can increase or reduce, but the quality proportioning constant rate between each composition.
The present invention provides a kind of neoprene emulsifier, and raw material components are by weight, comprising: 2~6 weight of rosin raw material
Part, 14~20 parts by weight of hydroxide and/or 1 parts by weight of hydroxide aqueous solution and deionized water；
Wherein, rosin raw material is rosin and/or disproportionated rosin；
Hydroxide is potassium hydroxide；Hydroxide aqueous solution is sodium hydroxide solution；Preferably, sodium hydroxide solution
Mass concentration is 30%~34%.
In further embodiment of the invention, the preparation method of rosin raw material is comprising steps of by masson pine rosin, answer
Antioxidant and solvent pinane are closed with 1:(0.4~0.5): the mass ratio of (0.02~0.03) is uniformly mixed, and is then dissolved by heating, is obtained
To mixed solution；Mixed solution is added in distilling apparatus, adjusts vacuum degree to 0.09~0.1MPa, then with 0.5~0.6
DEG C/heating rate of min is heated to 200~205 DEG C, after keeping the temperature 35~40min, closes vacuum, inert gas is filled with to distilling
Pressure in device is zero；Open vacuum, adjust distilling apparatus in vacuum degree be 80~120Pa, then with 0.01~0.02 DEG C/
The heating rate of min is warming up to 219~220 DEG C, and heat preservation 45~48min of distillation closes vacuum, is filled with inert gas to distilling dress
Pressure in setting is zero, and collection evaporates excess, obtains rosin raw material；Wherein, composite antioxidant include mass ratio be 1:(0.2~
0.3) antioxidant MB and antioxidant DNP.
In addition, including the following steps: the present invention also provides the preparation method of above-mentioned neoprene emulsifier
Nitrogen envelope is carried out to preparing tank injection nitrogen, is then injected into deionized water, opens exhaust-valve, turn on agitator, by matching
Than hydroxide and/or hydroxide aqueous solution is added；Wherein, when hydroxide is potassium hydroxide, potassium hydroxide time control is added
Adding rate processed is 19.5~20.5kg/min, preferably 20kg/min；
Alkali content (pH value is 10~11, and alkali content is 4.5%~5.0%) is measured by sampling after stirring 4~6min, detection is closed
Steam valve is opened after lattice to heat up；
Rosin raw material is proportionally added into preparing tank by electric block, closes exhaust-valve after adding material；
After temperature rises to 92 DEG C timing keep the temperature, and give preparing tank injection nitrogen carry out nitrogen envelope, according to temperature adjust steam into
Amount maintains 92 ± 1 DEG C always, keeps the temperature 5 hours；Wherein, sample detection solid content after timing keeps the temperature 2 hours stops when by 4 hours
Stirring, the 5th hour the second solid content of sample detection；Wherein, when hydroxide is potassium hydroxide, the corresponding potash soap of the second solid content
Solid content is 25 ± 0.5%；When hydroxide aqueous solution is sodium hydroxide solution, the corresponding soda soap solid content of the second solid content is
15 ± 0.5%；
After detection is qualified, cooling water circulating pump is opened, recirculated cooling water cooling is opened, is pumped to holding vessel when being down to 50 DEG C
It saves；When there is new prepared rosin soap (neoprene emulsifier) to squeeze into, holding vessel circulating pump is opened, material is carried out equal
Change, guarantees rosin soap uniform quality；Product is pumped into tank car according to user's dosage, and user's use is sent after weighing.
Neoprene emulsifier provided by the invention and preparation method thereof is made furtherly combined with specific embodiments below
It is bright.
Embodiment 1
The present embodiment provides a kind of neoprene emulsifier (rosin sodium soap), raw material components include: rosin 2.47kg, hydrogen-oxygen
Change sodium solution 1kg and deionized water 14.65kg；Wherein, the mass concentration of sodium hydroxide solution is 32%.
Neoprene emulsifier (rosin sodium soap) is prepared using preparation method provided by the invention by above-mentioned raw material:
Nitrogen envelope is carried out to preparing tank injection nitrogen, is then injected into deionized water, opens exhaust-valve, turn on agitator, by matching
Than sodium hydroxide solution is added；
Alkali content (pH value is 10~11, and alkali content is 4.5%~5.0%) is measured by sampling after stirring 5min, detection is qualified
Steam valve is opened afterwards to heat up；
Rosin is proportionally added into preparing tank by electric block, closes exhaust-valve after adding material；
After temperature rises to 92 DEG C timing keep the temperature, and give preparing tank injection nitrogen carry out nitrogen envelope, according to temperature adjust steam into
Amount maintains 92 ± 1 DEG C always, keeps the temperature 5 hours；Wherein, sample detection solid content after timing keeps the temperature 2 hours stops when by 4 hours
Stirring, the 5th hour the second solid content of sample detection (soda soap solid content) be 15 ± 0.5%；
After detection is qualified, cooling water circulating pump is opened, recirculated cooling water cooling is opened, is pumped to holding vessel when being down to 50 DEG C
It saves；When there is new prepared rosin sodium soap (neoprene emulsifier) to squeeze into, holding vessel circulating pump is opened, material is carried out
Homogenizing guarantees rosin sodium soap uniform quality；Product is pumped into tank car according to user's dosage, and user's use is sent after weighing.
Embodiment 2
The present embodiment provides a kind of neoprene emulsifiers (disproportionated rosin potassium soap), and raw material components include: disproportionated rosin
5.48kg, potassium hydroxide 1kg and deionized water 18.71kg.
Neoprene emulsifier (disproportionated rosin potassium is prepared using preparation method provided by the invention by above-mentioned raw material
Soap):
Nitrogen envelope is carried out to preparing tank injection nitrogen, is then injected into deionized water, opens exhaust-valve, turn on agitator, by matching
Than potassium hydroxide is added, control adding rate is 20kg/min when adding potassium hydroxide；
Alkali content (pH value is 10~11, and alkali content is 4.5%~5.0%) is measured by sampling after stirring 5min, detection is qualified
Steam valve is opened afterwards to heat up；
Disproportionated rosin is proportionally added into preparing tank by electric block, closes exhaust-valve after adding material；
After temperature rises to 92 DEG C timing keep the temperature, and give preparing tank injection nitrogen carry out nitrogen envelope, according to temperature adjust steam into
Amount maintains 92 ± 1 DEG C always, keeps the temperature 5 hours；Wherein, sample detection solid content after timing keeps the temperature 2 hours stops when by 4 hours
Stirring, the 5th hour the second solid content of sample detection (potash soap solid content) be 25 ± 0.5%；
After detection is qualified, cooling water circulating pump is opened, recirculated cooling water cooling is opened, is pumped to holding vessel when being down to 50 DEG C
It saves；When there is new prepared disproportionated rosin potassium soap (neoprene emulsifier) to squeeze into, holding vessel circulating pump is opened, by material
It is homogenized, guarantees disproportionated rosin potassium soap uniform quality；Product is pumped into tank car according to user's dosage, and user's use is sent after weighing i.e.
It can.
Embodiment 3
The present embodiment provides a kind of neoprene emulsifier (rosin sodium soap), raw material components include: rosin 2.47kg, hydrogen-oxygen
Change sodium solution 1kg and deionized water 14.65kg；Wherein, the mass concentration of sodium hydroxide solution is 32%；
Wherein, the preparation method of rosin is comprising steps of by masson pine rosin, composite antioxidant and solvent pinane with 1:
The mass ratio of 0.45:0.025 is uniformly mixed, and is then dissolved by heating, is obtained mixed solution；Distilling apparatus is added in mixed solution
In, then adjustment vacuum degree to 0.095MPa is heated to 202 DEG C with the heating rate of 0.55 DEG C/min, after keeping the temperature 38min, close
Vacuum is closed, being filled with pressure of the inert gas into distilling apparatus is zero；Vacuum is opened, adjusting vacuum degree in distilling apparatus is
100Pa, is then warming up to 220 DEG C with the heating rate of 0.016 DEG C/min, and heat preservation distillation 46min closes vacuum, is filled with inertia
Pressure of the gas into distilling apparatus is zero, and collection evaporates excess, obtains rosin；Wherein, it is 1 that composite antioxidant, which includes mass ratio:
0.24 antioxidant MB and antioxidant DNP.
Neoprene emulsifier (rosin sodium soap) is prepared using preparation method provided by the invention by above-mentioned raw material:
Nitrogen envelope is carried out to preparing tank injection nitrogen, is then injected into deionized water, opens exhaust-valve, turn on agitator, by matching
Than sodium hydroxide solution is added；
Alkali content (pH value is 10~11, and alkali content is 4.5%~5.0%) is measured by sampling after stirring 5min, detection is qualified
Steam valve is opened afterwards to heat up；
Rosin is proportionally added into preparing tank by electric block, closes exhaust-valve after adding material；
After temperature rises to 92 DEG C timing keep the temperature, and give preparing tank injection nitrogen carry out nitrogen envelope, according to temperature adjust steam into
Amount maintains 92 ± 1 DEG C always, keeps the temperature 5 hours；Wherein, sample detection solid content after timing keeps the temperature 2 hours stops when by 4 hours
Stirring, the 5th hour the second solid content of sample detection (soda soap solid content) be 15 ± 0.5%；
After detection is qualified, cooling water circulating pump is opened, recirculated cooling water cooling is opened, is pumped to holding vessel when being down to 50 DEG C
It saves；When there is new prepared rosin sodium soap (neoprene emulsifier) to squeeze into, holding vessel circulating pump is opened, material is carried out
Homogenizing guarantees rosin sodium soap uniform quality；Product is pumped into tank car according to user's dosage, and user's use is sent after weighing.
Comparative example 1
This comparative example provides a kind of neoprene emulsifier (rosin sodium soap), and raw material components include: rosin 2.47kg, hydrogen-oxygen
Change sodium solution 1kg and deionized water 14.65kg；Wherein, the mass concentration of sodium hydroxide solution is 32%；
Wherein, the preparation method of rosin is comprising steps of masson pine rosin and solvent pinane are mixed with the mass ratio of 1:0.025
It closes uniformly, then dissolves by heating, obtain mixed solution；Mixed solution is added in distilling apparatus, adjustment vacuum degree is extremely
Then 0.095MPa is heated to 202 DEG C with the heating rate of 0.55 DEG C/min, after keeping the temperature 38min, close vacuum, be filled with inertia
Pressure of the gas into distilling apparatus is zero；Vacuum is opened, adjusting vacuum degree in distilling apparatus is 100Pa, then with 0.016
DEG C/heating rate of min is warming up to 220 DEG C, heat preservation distillation 46min closes vacuum, is filled with inert gas into distilling apparatus
Pressure is zero, and collection evaporates excess, obtains rosin.
By above-mentioned raw material, neoprene emulsifier (rosin sodium soap) is prepared:
Nitrogen envelope is carried out to preparing tank injection nitrogen, is then injected into deionized water, opens exhaust-valve, turn on agitator, by matching
Than sodium hydroxide solution is added；
Alkali content (pH value is 10~11, and alkali content is 4.5%~5.0%) is measured by sampling after stirring 5min, detection is qualified
Steam valve is opened afterwards to heat up；
Rosin is proportionally added into preparing tank by electric block, closes exhaust-valve after adding material；
After temperature rises to 92 DEG C timing keep the temperature, and give preparing tank injection nitrogen carry out nitrogen envelope, according to temperature adjust steam into
Amount maintains 92 ± 1 DEG C always, keeps the temperature 5 hours；Wherein, sample detection solid content after timing keeps the temperature 2 hours stops when by 4 hours
Stirring, the 5th hour the second solid content of sample detection (soda soap solid content) be 15 ± 0.5%；
After detection is qualified, cooling water circulating pump is opened, recirculated cooling water cooling is opened, is pumped to holding vessel when being down to 50 DEG C
It saves；When there is new prepared rosin sodium soap (neoprene emulsifier) to squeeze into, holding vessel circulating pump is opened, material is carried out
Homogenizing guarantees rosin sodium soap uniform quality；Product is pumped into tank car according to user's dosage, and user's use is sent after weighing.
Comparative example 2
This comparative example provides a kind of neoprene emulsifier (rosin sodium soap), and raw material components include: rosin 2.47kg, hydrogen-oxygen
Change sodium solution 1kg and deionized water 14.65kg；Wherein, the mass concentration of sodium hydroxide solution is 32%；
Wherein, the preparation method of rosin is comprising steps of by masson pine rosin, composite antioxidant and solvent pinane with 1:
The mass ratio of 0.45:0.025 is uniformly mixed, and is then dissolved by heating, is obtained mixed solution；Distilling apparatus is added in mixed solution
In, then adjustment vacuum degree to 0.095MPa is heated to 202 DEG C with the heating rate of 0.55 DEG C/min, after keeping the temperature 38min, close
Vacuum is closed, being filled with pressure of the inert gas into distilling apparatus is zero；Vacuum is opened, adjusting vacuum degree in distilling apparatus is
100Pa, is then warming up to 220 DEG C with the heating rate of 0.016 DEG C/min, and heat preservation distillation 46min closes vacuum, is filled with inertia
Pressure of the gas into distilling apparatus is zero, and collection evaporates excess, obtains rosin；Wherein, it is 1 that composite antioxidant, which includes mass ratio:
0.24 antioxidant MB and antioxidant DNP.
By above-mentioned raw material, neoprene emulsifier (rosin sodium soap) is prepared:
Nitrogen envelope is carried out to preparing tank injection nitrogen, is then injected into deionized water, opens exhaust-valve, turn on agitator, by matching
Than sodium hydroxide solution is added；
Alkali content (pH value is 10~11, and alkali content is 4.5%~5.0%) is measured by sampling after stirring 5min, detection is qualified
Steam valve is opened afterwards to heat up；
Rosin is proportionally added into preparing tank by electric block, closes exhaust-valve after adding material；
After temperature rises to 95 DEG C timing keep the temperature, and give preparing tank injection nitrogen carry out nitrogen envelope, according to temperature adjust steam into
Amount maintains 95 ± 1 DEG C always, keeps the temperature 5 hours；Wherein, sample detection solid content after timing keeps the temperature 2 hours stops when by 4 hours
Stirring, the 5th hour the second solid content of sample detection (soda soap solid content) be 15 ± 0.5%；
After detection is qualified, cooling water circulating pump is opened, recirculated cooling water cooling is opened, is pumped to holding vessel when being down to 50 DEG C
It saves；When there is new prepared rosin sodium soap (neoprene emulsifier) to squeeze into, holding vessel circulating pump is opened, material is carried out
Homogenizing guarantees rosin sodium soap uniform quality；Product is pumped into tank car according to user's dosage, and user's use is sent after weighing.
The neoprene emulsifier that the embodiment of the present invention 1 to embodiment 3 is prepared, by function assessment test come system
Its effect is evaluated, and using the neoprene emulsifier that comparative example 1 and comparative example 2 are prepared as control.
Prepare modified chloroprene rubber: (1) raw material components are by weight, comprising: 54 parts by weight of neoprene, natural rubber
26 parts by weight, 2.1 parts by weight of magnesia, 0.8 parts by weight of zinc oxide, 1.2 parts of promotor, 2 parts by weight of vulcanizing agent, stearic acid 1.0
Parts by weight, 4 parts by weight of adhesive, 14 parts by weight of carbon black, adjacent 4 parts by weight of dibutyl ester and 11 parts by weight of emulsifier.Emulsifier is this
Neoprene rubber is prepared in the neoprene emulsifier or comparative example 1 to comparative example 2 that inventive embodiments 1 to embodiment 3 is prepared
Latex agent.(2) preparation method is comprising steps of S1: raw rubber is plasticated: neoprene and natural rubber are sent into kneading machine,
It plasticates under the conditions of 38.6 DEG C, is uniformly mixed and obtains broken-down rubber, storage period 12h, standby be kneaded is used；S2: it is kneaded: successively will be stearic
Acid, zinc oxide, magnesia, adhesive A, carbon black, adjacent dibutyl ester and emulsifier are added in the broken-down rubber after parking, in kneading machine
In be kneaded under the conditions of 110 DEG C, obtain rubber compound；S3: vulcanization: rubber compound and other surplus stock components are added to
In EK2000 type vulcameter, vulcanizes 26min under the conditions of 0.5MPa, 172 DEG C, obtain modified chloroprene rubber.
The Modified Polychloroprene rubber that the neoprene emulsifier being prepared using embodiment 1-3, comparative example 1-2 is prepared
The performance indicator of glue and commercially available neoprene detects, and the results are shown in Table 1.As can be seen from the results, using 1-3 of the embodiment of the present invention
The modified chloroprene rubber that the neoprene emulsifier of offer is prepared relative to traditional commercially available neoprene and uses this hair
The modified chloroprene rubber that the neoprene emulsifier that bright comparative example 1-2 is provided is prepared, hardness with higher are pulled apart strong
Degree, elasticity are more preferable, and brittle temperature reduces, and have high rigidity and high cold resistance.
1 testing result of table
| Performance indicator | Shore hardness A/ degree | Breaking strength/MPa | Elongation at break/% | Brittle temperature/DEG C |
| Embodiment 1 | 77 | 26.3 | 872 | -54 |
| Embodiment 2 | 78 | 26.7 | 864 | -52 |
| Embodiment 3 | 82 | 29.4 | 893 | -59 |
| Comparative example 1 | 68 | 17.9 | 826 | -42 |
| Comparative example 2 | 63 | 18.3 | 847 | -48 |
| Commercially available neoprene | 60 | 15.1 | 810 | -36 |
It should be noted that unless otherwise indicated, technical term or scientific term used in this application should be this hair
The ordinary meaning that bright one of ordinary skill in the art are understood.Unless specifically stated otherwise, it otherwise illustrates in these embodiments
Component and opposite step, numerical expression and the numerical value of step are not limit the scope of the invention.It is illustrated and described herein
In all examples, unless otherwise prescribed, any occurrence should be construed as merely illustratively, not as limitation, because
This, other examples of exemplary embodiment can have different values.
In the description of the present invention, it is to be understood that, term " first ", " second " are used for description purposes only, and cannot
It is interpreted as indication or suggestion relative importance or implicitly indicates the quantity of indicated technical characteristic.Define as a result, " the
One ", the feature of " second " can explicitly or implicitly include one or more of the features.In the description of the present invention,
The meaning of " plurality " is two or more, unless otherwise specifically defined.
Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations；To the greatest extent
Pipe present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: its according to
So be possible to modify the technical solutions described in the foregoing embodiments, or to some or all of the technical features into
Row equivalent replacement；And these are modified or replaceed, various embodiments of the present invention technology that it does not separate the essence of the corresponding technical solution
The range of scheme should all cover in protection scope of the present invention.
Claims (10)
1. a kind of neoprene emulsifier, which is characterized in that raw material components are by weight, comprising:
14~20 weight of 2~6 parts by weight of rosin raw material, hydroxide and/or 1 parts by weight of hydroxide aqueous solution and deionized water
Part.
2. neoprene emulsifier according to claim 1, it is characterised in that:
The rosin raw material is rosin and/or disproportionated rosin.
3. neoprene emulsifier according to claim 1, it is characterised in that:
The hydroxide is potassium hydroxide；
The hydroxide aqueous solution is sodium hydroxide solution；Preferably, the mass concentration of the sodium hydroxide solution is 30%
~34%.
4. neoprene emulsifier according to claim 1, which is characterized in that raw material components are by weight, comprising:
18.71 parts by weight of 5.48 parts by weight of disproportionated rosin, 1 parts by weight of potassium hydroxide and deionized water.
5. neoprene emulsifier according to claim 1, which is characterized in that raw material components are by weight, comprising:
14.65 parts by weight of 2.47 parts by weight of rosin, 1 parts by weight of sodium hydroxide solution and deionized water；
Wherein, the mass concentration of the sodium hydroxide solution is 32%.
6. neoprene emulsifier according to claim 1, which is characterized in that the preparation method of the rosin raw material includes
Step:
Masson pine rosin, composite antioxidant and solvent are uniformly mixed, then dissolved by heating, mixed solution is obtained；
The mixed solution is added in distilling apparatus, vacuum degree is adjusted to 0.09~0.1MPa, is then heated to 200~205
DEG C, after keeping the temperature 35~40min, vacuum is closed, being filled with pressure of the inert gas into distilling apparatus is zero；
Vacuum is opened, adjusting vacuum degree in distilling apparatus is 80~120Pa, then heats to 219~220 DEG C, heat preservation distillation 45
~48min closes vacuum, and being filled with pressure of the inert gas into distilling apparatus is zero, and collection evaporates excess, and it is former to obtain the rosin
Material.
7. neoprene emulsifier according to claim 6, it is characterised in that:
The composite antioxidant includes antioxidant MB and antioxidant DNP；The mass ratio of the antioxidant MB and the antioxidant DNP
For 1:(0.2~0.3)；
The solvent is pinane.
8. neoprene emulsifier according to claim 6, it is characterised in that:
The mass ratio of the masson pine rosin, the composite antioxidant and the solvent is 1:(0.4~0.5): (0.02~
0.03)；
The heating rate for being heated to using during 200~205 DEG C is 0.5~0.6 DEG C/min；
The heating rate used during 219~220 DEG C that is warming up to is 0.01~0.02 DEG C/min.
9. the preparation method of the described in any item neoprene emulsifiers of claim 1-8, which is characterized in that comprising steps of
Carry out nitrogen envelope to preparing tank injection nitrogen, be then injected into deionized water, open exhaust-valve, turn on agitator, according to the ratio plus
Enter hydroxide and/or hydroxide aqueous solution；
Alkali content is measured by sampling after 4~6min of stirring, opens steam valve after detection is qualified and heats up；
Rosin raw material is proportionally added into preparing tank by electric block, closes exhaust-valve after adding material；
Timing is kept the temperature after temperature rises to 92 DEG C, and carries out nitrogen envelope to preparing tank injection nitrogen, is adjusted steam input according to temperature, is begun
92 ± 1 DEG C are maintained eventually, keep the temperature 5 hours；Wherein, sample detection solid content after timing keeps the temperature 2 hours stops stirring when by 4 hours,
5th hour the second solid content of sample detection；
After detection is qualified, cooling water circulating pump is opened, opens recirculated cooling water cooling, holding vessel guarantor is pumped to when being down to 50 DEG C
It deposits.
10. the preparation method of neoprene emulsifier according to claim 9, it is characterised in that:
When the hydroxide is potassium hydroxide, control adding rate is 19.5~20.5kg/min when adding potassium hydroxide, excellent
It is selected as 20kg/min；
The alkali content is 4.5%~5.0%, and pH value is 10~11；
When the hydroxide is potassium hydroxide, the corresponding potash soap solid content of second solid content is 25 ± 0.5%；
When the hydroxide aqueous solution is sodium hydroxide solution, the corresponding soda soap solid content of second solid content is 15 ±
0.5%.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2003052034A1 (en) * | 2001-12-17 | 2003-06-26 | Resitec Industria Quimica Ltda. | Process for separating saponifiable and non-saponifiable compounds comprised in a vegetable or animal raw material |
| CN103058857A (en) * | 2013-01-06 | 2013-04-24 | 二创（福建）化工科技有限公司 | Preparation method of disproportionated rosin potassium soap |
| CN107383508A (en) * | 2017-08-22 | 2017-11-24 | 浙江久运汽车零部件有限公司 | A kind of modified chloroprene rubber and preparation method thereof |
| CN107501441A (en) * | 2017-09-07 | 2017-12-22 | 宁波顺泽橡胶有限公司 | A kind of rubber production isproportionated potassium rosinate preparation method |
| CN107936845A (en) * | 2017-11-16 | 2018-04-20 | 高海娟 | The preparation method of rosin |
| CN108587472A (en) * | 2018-06-08 | 2018-09-28 | 南通米高电子科技有限公司 | A kind of preparation method of rosin |
-
2018
- 2018-10-09 CN CN201811172845.3A patent/CN109232911A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2003052034A1 (en) * | 2001-12-17 | 2003-06-26 | Resitec Industria Quimica Ltda. | Process for separating saponifiable and non-saponifiable compounds comprised in a vegetable or animal raw material |
| CN103058857A (en) * | 2013-01-06 | 2013-04-24 | 二创（福建）化工科技有限公司 | Preparation method of disproportionated rosin potassium soap |
| CN107383508A (en) * | 2017-08-22 | 2017-11-24 | 浙江久运汽车零部件有限公司 | A kind of modified chloroprene rubber and preparation method thereof |
| CN107501441A (en) * | 2017-09-07 | 2017-12-22 | 宁波顺泽橡胶有限公司 | A kind of rubber production isproportionated potassium rosinate preparation method |
| CN107936845A (en) * | 2017-11-16 | 2018-04-20 | 高海娟 | The preparation method of rosin |
| CN108587472A (en) * | 2018-06-08 | 2018-09-28 | 南通米高电子科技有限公司 | A kind of preparation method of rosin |
Non-Patent Citations (1)
| Title |
|---|
| 宋建国等: "《化工原理》", 31 July 2007, 东北林业大学出版社 * |
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