CN108080561A - A kind of heat curing type environment friendly curing agent and preparation method thereof - Google Patents
A kind of heat curing type environment friendly curing agent and preparation method thereof Download PDFInfo
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- CN108080561A CN108080561A CN201711096843.6A CN201711096843A CN108080561A CN 108080561 A CN108080561 A CN 108080561A CN 201711096843 A CN201711096843 A CN 201711096843A CN 108080561 A CN108080561 A CN 108080561A
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- acid
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- curing agent
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22C—FOUNDRY MOULDING
- B22C1/00—Compositions of refractory mould or core materials; Grain structures thereof; Chemical or physical features in the formation or manufacture of moulds
- B22C1/16—Compositions of refractory mould or core materials; Grain structures thereof; Chemical or physical features in the formation or manufacture of moulds characterised by the use of binding agents; Mixtures of binding agents
- B22C1/20—Compositions of refractory mould or core materials; Grain structures thereof; Chemical or physical features in the formation or manufacture of moulds characterised by the use of binding agents; Mixtures of binding agents of organic agents
- B22C1/22—Compositions of refractory mould or core materials; Grain structures thereof; Chemical or physical features in the formation or manufacture of moulds characterised by the use of binding agents; Mixtures of binding agents of organic agents of resins or rosins
- B22C1/2233—Compositions of refractory mould or core materials; Grain structures thereof; Chemical or physical features in the formation or manufacture of moulds characterised by the use of binding agents; Mixtures of binding agents of organic agents of resins or rosins obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- B22C1/224—Furan polymers
Abstract
The invention discloses a kind of heat curing type environment friendly curing agent and preparation method thereof, oleum carries out sulfonating reaction with dimethylbenzene (stupid) in the range of 150 DEG C 300 DEG C, and sulfonation time is controlled when 8-30 is small；Esterification is carried out with environmentally friendly solvent after product cooling, heat preservation after sulfonation, then carries out acidity adjustment.Curing agent prepared by the present invention is suitble to heat cure, and normal temperature cure speed is slow, there is a sufficient up time, and curing rate is fast during heating.(the molding sand usage time of preparation is long then reusable) reusable after sand reclamation after hardening, will not cause secondary pollution.The compactness of the accuracy of casting, surface quality and material is all greatly improved simultaneously.
Description
Technical field
The present invention relates to curing agent technical fields, particularly relate to a kind of heat curing type environment friendly curing agent and preparation method thereof, should
Curing agent can be used for the production of cast steel, cast iron and non-ferrous metal.
Background technology
Molding sand is the material for being used for moulding in sand casting, and molding sand is generally by casting model powder, moulding sand binder and additional thing
Modeling Materials is waited to mix according to a certain percentage.Adhesive generates firm bonding between the particle of sand, assigns molding sand institute
Required mechanical stability.Additional thing such as curing agent energy speed adhesive cures.
P-methyl benzenesulfonic acid is used to synthesize in medicine the important source material of fortimicin, amoxicillin intermediate etc.；Organic
The catalyst of textile auxiliary, photographic film, the stabilizer of polymerisation and organic synthesis esters is widely used in chemical industry；
The industries such as resin, coating, wood-based plate, casting are widely used as curing agent, and curing rate is fast, and paint film is non-discolouring.
In industrial production, the concentrated sulfuric acid of toluene and excess generates the mixed liquor of p-methyl benzenesulfonic acid and sulfuric acid in a kettle
Body, mixed liquor crystallisation by cooling in crystallization tank, which is put into centrifuge, to be separated, and crystal is p-methyl benzenesulfonic acid, and the liquid thrown away is
Sulfonic acid mother liquor body, partial modulation curing agent are sold, and partly reaction generates toluenesulfonic acid sodium salt liquid, liquid in and in pot with liquid base
Body is that toluenesulfonic acid sodium salt solid is sold after heavy salt concentration of decolourizing centrifuges or is spray-dried.
But p-methyl benzenesulfonic acid curing agent is present with the problem of finished product total acid number and higher free acid value in production, influences
The service efficiency of curing agent, and existing sulfonic acid curing agent preparation time is longer, and generation wastewater flow rate is more, production efficiency and environmental protection
It is it is required that all undesirable.
Previous p-methyl benzenesulfonic acid is used as curing furane resins, is normal temperature cure, the up time of molding sand is 10-30 (60)
Minute.Because the up time is short, (jar) blasting unit will be solidificated in by running into specific question even work shift problem, sand
In lead to not to penetrate the deuce to pay of sand processing.
The content of the invention
The purpose of the present invention aiming at the above-mentioned prior art situation, in order to solve existing curing agent total acid number with it is free
The problems such as acid value is higher, and molding sand normal temperature cure usage time is short, the present invention disclose a kind of heat curing type environment friendly curing agent and its preparation
Method.
The purpose of the present invention is what is be achieved through the following technical solutions：A kind of heat curing type environment friendly curing agent, including diformazan
Benzene, oleum, environmentally friendly solvent and inorganic acid；
The environmentally friendly solvent includes one or more combinations in phosphoric acid, oleic acid or dipropylene glycol methyl ether；
The curing agent component formula is calculated as with parts by weight：840-860 parts of dimethylbenzene, 1040-1060 parts of oleum,
30-150 parts of 560-950 parts of environmentally friendly solvent and inorganic acid.
Further, the raw material of following parts by weight is included：860 parts of dimethylbenzene, 1060 parts of oleum, environmentally friendly solvent 1500
150 parts of part and inorganic acid.
Further, the environmentally friendly solvent is the combination of phosphoric acid, oleic acid and dipropylene glycol methyl ether, and component formula is with weight
Number is calculated as：130-300 parts of 30-300 parts of phosphatase 11,300-350 parts of oleic acid and dipropylene glycol methyl ether.
1. further, the environmentally friendly solvent is the combination of phosphoric acid and dipropylene glycol methyl ether, component formula is with parts by weight
Number is calculated as：300-600 parts of phosphoric acid, 260-350 parts of dipropylene glycol methyl ether.
Further, the inorganic acid for dimethyl carbonate, hydrochloric acid, sulfuric acid, nitric acid, boric acid, phosphoric acid, pyrophosphoric acid, carbonic acid,
One or more combinations in formic acid, acetic acid, fat polyacid class, fragrant acids or fragrant polyacid class.
A kind of preparation method of heat curing type environment friendly curing agent, comprises the following steps：
Step 1：Raw material is weighed by parts by weight component formula described in claim 1,
Step 2：Dimethylbenzene is added in into reaction kettle, oleum, which is added dropwise, when being warming up to 150 DEG C~300 DEG C carries out sulphur
Change reaction, when the sulfonating reaction time 8~30 is small,
Step 3：Temperature 50 C~80 DEG C are cooled to, when heat preservation 0.5~1.5 is small,
Step 4：Product after sulfonating reaction carries out esterification, adds in environmentally friendly solvent,
Step 5：30 DEG C~60 DEG C are cooled to, adds in inorganic acid, acidity is adjusted to 5~18.
Further, the inorganic acid for dimethyl carbonate, hydrochloric acid, sulfuric acid, nitric acid, boric acid, phosphoric acid, pyrophosphoric acid, carbonic acid,
One or more combinations in formic acid, acetic acid, fat polyacid class, fragrant acids or fragrant polyacid class.
Further, the environmentally friendly solvent is one or more combinations in phosphoric acid, oleic acid or dipropylene glycol methyl ether.
The beneficial effects of the present invention are：
1. carry out esterification to product again after sulfonating reaction, the free acid in curing agent is reduced, after simultaneous reactions
A kind of ingredient of the component as curing agent, can further play curing function.
2. removing the sulphur in product by esterification, the harmful substance of cast steel is reduced.
3. by esterification and adjusting acidity, curing agent is made to extend hardening time in application, reach slowly cured
Effect increases the up time of molding sand.
4. waterglass is replaced to lose the shell moulded casting of wax：Waterglass, which loses wax shell mold casting, needs 7-10 days, and applies the present invention
Product then only need 3-5 minutes, the time greatly shortens；Waterglass loses wax shell mold casting pollution environment, shell cannot degrade；Using this
Then the cycle is short for the product of invention, and cost reduction 50%, after casting, reclaimed sand is reusable, will not cause secondary pollution；Simultaneously
The compactness of the accuracy of casting, surface quality and material is all greatly improved.
Specific embodiment
It, below will be to the skill in the embodiment of the present application in order to which those skilled in the art is made to more fully understand application scheme
Art scheme is clearly and completely described, it is clear that and described embodiment is only the embodiment of the application part, without
It is whole embodiments.Based on the embodiment in the application, those of ordinary skill in the art are not before creative work is made
All other embodiments obtained are put, should all belong to the scope of the application protection.
A kind of heat curing type environment friendly curing agent of the present invention, including dimethylbenzene, oleum, environmentally friendly solvent and inorganic acid；
The environmentally friendly solvent includes one or more combinations in phosphoric acid, oleic acid or dipropylene glycol methyl ether.Phosphoric acid can reduce
Organic acid total amount, sulfonic acid curing rate is fast and phosphoric acid curing rate is slowly easy to control, improves the feature of environmental protection；Oleic acid plays the work of releasing agent
With being conducive to molding, reduce sand and mold adhesion, guarantee type integrality, oleic acid is also acid, cures and is easy to so also functioning to
Molding effect；Dipropylene glycol methyl ether is hypotoxicity, low viscosity, the colourless transparent liquid of low surface tension.Its evaporation rate is fitted
Degree has good dissolving, coupling capacity.Since its is miscible with water, there is appropriate HLB value, can dissolve grease, natural resin
With rubber, cellulose, polyvinyl acetate, polyvinyl alcohol contracting first/second/butyraldehyde, alkyd resin, phenolic resin, urea resin etc.
Polymer chemistry substance.
The inorganic acid is dimethyl carbonate, hydrochloric acid, sulfuric acid, nitric acid, boric acid, phosphoric acid, pyrophosphoric acid, carbonic acid, formic acid, second
One or more combinations in acid, fat polyacid class, fragrant acids or fragrant polyacid class.The inorganic acid of addition plays diluting effect, can incite somebody to action
Acidity is transferred to 5-18.
The component formula of the present invention is calculated as with parts by weight：840-860 parts of dimethylbenzene, 1040-1060 parts of oleum, ring
Protect 30-150 parts of 560-9500 parts of solvent and inorganic acid.
A kind of preparation method of heat curing type environment friendly curing agent, comprises the following steps：
Step 1：Number component formula weighs raw material according to required weight,
Step 2：Dimethylbenzene is added in into reaction kettle, oleum, which is added dropwise, when being warming up to 150 DEG C~300 DEG C carries out sulphur
Change reaction, when the sulfonating reaction time 8~30 is small,
Step 3：Temperature 50 C~80 DEG C are cooled to, when heat preservation 0.5~1.5 is small,
Step 4：Product after sulfonating reaction adds in environmentally friendly solvent and carries out esterification, and esterification purpose one is to reduce sulphur pair
The influence of cast steel reduces harmful substance；Second is that reducing acidity, molding sand is made slowly to cure, improve up time and intensity.Ether and
Ester forms ethyl-sulfate and a kind of curing agent, while reduces free acid, be easy to cure and control.Meanwhile sand can be used when
Between also increase.
Step 5：30 DEG C~60 DEG C are cooled to, adds in inorganic acid, acidity is adjusted to 5~18.
Embodiment 1
A kind of preparation method of heat curing type environment friendly curing agent, comprises the following steps：
Step 1：840 parts of component dimethylbenzene, 1040 parts of oleum, 30 parts of phosphatase 11,300 parts of oleic acid, dipropyl by weight
130 parts of glycol methyl ether and 30 parts of component formulas of dimethyl carbonate weigh raw material,
Step 2：Dimethylbenzene is added in into reaction kettle, it is anti-that oleum progress sulfonation is added dropwise when being warming up to 150 DEG C DEG C
Should, when the sulfonating reaction time 8 is small,
Step 3：Temperature 50 C is cooled to, when heat preservation 0.5 is small,
Step 4：Product after sulfonating reaction adds in phosphoric acid, oleic acid, dipropylene glycol methyl ether and carries out esterification,
Step 5：30 DEG C are cooled to, adds in dimethyl carbonate, acidity is adjusted to 5.Ether and ester can be formed ethyl-sulfate and
A kind of curing agent, while reduce free acid, be easy to cure and control.Meanwhile the sand up time also increases.
Embodiment 2
A kind of preparation method of heat curing type environment friendly curing agent, comprises the following steps：
Step 1：860 parts of component dimethylbenzene, 1060 parts of oleum, 300 parts of phosphoric acid, 350 parts of oleic acid, dipropyl by weight
350 parts of glycol methyl ether and 150 parts of component formulas of dimethyl carbonate weigh raw material,
Step 2：Dimethylbenzene is added in into reaction kettle, oleum, which is added dropwise, when being warming up to 300 DEG C carries out sulfonating reaction,
When the sulfonating reaction time 30 is small,
Step 3：Temperature is cooled to 80 DEG C, when heat preservation 1.5 is small,
Step 4：Product after sulfonating reaction adds in phosphoric acid, oleic acid, dipropylene glycol methyl ether and carries out esterification,
Step 5：60 DEG C are cooled to, adds in dimethyl carbonate, acidity is adjusted to 18.
Embodiment 3
A kind of preparation method of heat curing type environment friendly curing agent, comprises the following steps：
Step 1：850 parts of component dimethylbenzene, 1050 parts of oleum, 260 parts of dipropylene glycol methyl ether and phosphoric acid by weight
300 parts of component formulas weigh raw material,
Step 2：Dimethylbenzene is added in into reaction kettle, oleum, which is added dropwise, when being warming up to 250 DEG C carries out sulfonating reaction,
When the sulfonating reaction time 20 is small,
Step 3：Temperature is cooled to 60 DEG C, when heat preservation 1.0 is small,
Step 4：Product after sulfonating reaction adds in oleic acid, dipropylene glycol methyl ether carries out esterification,
Step 5：50 DEG C are cooled to, adds in phosphoric acid, acidity is adjusted to 12.
Previous sulfonic acid is used as curing furane resins, and the sand up time is 10-60 minutes, it is normal temperature cure, the present invention
Heat cure, the sand up time reach 24-60 it is small when.If the up time is short, specific question even shift is run into
Secondary problem, sand will be solidificated in the deuce to pay for leading to not processing in jar.The inventive point of the present invention is exactly to pass through to adjust acid,
Sand reach 24-60 it is small when up time.The purpose of esterification is exactly acidity reduction, improves up time and intensity.I.e.：
Sulfonic acid is rapid curing, and for the present invention slowly to cure, the up time is long.Waterglass can further be replaced to lose the shell mould casting of wax
It makes：Waterglass, which loses wax shell mold casting, needs 7-10 days, and the product of the present invention is applied then only to need 3-5 minutes, and the time greatly shortens；
Waterglass loses wax shell mold casting pollution environment, shell cannot degrade；Using product of the invention, then the cycle is short, cost reduction 50%,
After casting, reclaimed sand is reusable, will not cause secondary pollution；The cause of the accuracy of casting, surface quality and material simultaneously
Close property is all greatly improved.
Above-mentioned the embodiment of the present application sequence number is for illustration only, does not represent the quality of embodiment.
The above is only the preferred embodiment of the application, it is noted that for the ordinary skill people of the art
For member, on the premise of the application principle is not departed from, several improvements and modifications can also be made, these improvements and modifications also should
It is considered as the protection domain of the application.
Claims (8)
1. a kind of heat curing type environment friendly curing agent, which is characterized in that including dimethylbenzene, oleum, environmentally friendly solvent and inorganic acid；Its
In,
The environmentally friendly solvent includes one or more combinations in phosphoric acid, oleic acid or dipropylene glycol methyl ether；
The curing agent component formula is calculated as with parts by weight：840-860 parts of dimethylbenzene, 1040-1060 parts of oleum, environmental protection
30-150 parts of 560-950 parts of solvent and inorganic acid.
2. heat curing type environment friendly curing agent as described in claim 1, which is characterized in that include the raw material of following parts by weight：Diformazan
150 parts of 860 parts of benzene, 1060 parts of oleum, 560 parts of environmentally friendly solvent and inorganic acid.
3. heat curing type environment friendly curing agent as described in claim 1, which is characterized in that the environmentally friendly solvent for phosphoric acid, oleic acid and
The combination of dipropylene glycol methyl ether, component formula are calculated as with parts by weight：30-300 parts of phosphatase 11,300-350 parts of oleic acid and dipropyl
130-300 parts of glycol methyl ether.
4. heat curing type environment friendly curing agent as described in claim 1, which is characterized in that the environmentally friendly solvent is phosphoric acid and dipropyl two
The combination of alcohol methyl ether, component formula are calculated as with parts by weight：300-600 parts of phosphoric acid, 260-350 parts of dipropylene glycol methyl ether.
5. heat curing type environment friendly curing agent as described in claim 1, which is characterized in that the inorganic acid is dimethyl carbonate, salt
In acid, sulfuric acid, nitric acid, boric acid, phosphoric acid, pyrophosphoric acid, carbonic acid, formic acid, acetic acid, fat polyacid class, fragrant acids or fragrant polyacid class
One or more combination.
6. a kind of preparation method of heat curing type environment friendly curing agent, which is characterized in that comprise the following steps：
Step 1：Raw material is weighed by parts by weight component formula described in claim 1,
Step 2：Dimethylbenzene is added in into reaction kettle, it is anti-that oleum progress sulfonation is added dropwise when being warming up to 150 DEG C~300 DEG C
Should, when the sulfonating reaction time 8~30 is small,
Step 3：Temperature 50 C~80 DEG C are cooled to, when heat preservation 0.5~1.5 is small,
Step 4：Product after sulfonating reaction carries out esterification, adds in environmentally friendly solvent,
Step 5：30 DEG C~60 DEG C are cooled to, adds in inorganic acid, acidity is adjusted to 5~18.
A kind of preparation method of heat curing type environment friendly curing agent according to claim 2, feature is in the environmentally friendly solvent is
One or more combinations in phosphoric acid, oleic acid or dipropylene glycol methyl ether.
7. a kind of preparation method of heat curing type environment friendly curing agent according to claim 6, feature is in the inorganic acid is
Dimethyl carbonate, hydrochloric acid, sulfuric acid, nitric acid, boric acid, phosphoric acid, pyrophosphoric acid, carbonic acid, formic acid, acetic acid, fat polyacid class, fragrant acids or
One or more combinations in fragrant polyacid class.
8. a kind of preparation method of heat curing type environment friendly curing agent according to claim 6, feature is in the environmentally friendly solvent
For the one or more combination in phosphoric acid, oleic acid or dipropylene glycol methyl ether.
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Cited By (1)
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| CN110614342A (en) * | 2019-10-24 | 2019-12-27 | 福建省同兴汽车同步器有限公司石狮鸿山分公司 | Regenerative casting precoated sand using waste sand as raw material and preparation process thereof |
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