CN103113548A - Preparation method of novel modified furan resin for casting - Google Patents
Preparation method of novel modified furan resin for casting Download PDFInfo
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Abstract
The invention discloses a preparation method of novel modified furan resin for casting. The method is characterized by comprising the following steps of: (1) dissolving 100 parts by weight of saccharides and 0.1-40 parts by weight of urea into 30-200 parts by weight of water; adding 5-60 parts by weight of acid into a mixture to react for 0.5-10 hours at the temperature of 60-105 DEG C; cooling to 30-90 DEG C; regulating a pH value to 7.5-10 and adding 0.1-40 parts by weight of formaldehyde; raising the temperature to 60-100 DEG C to react for 0.5-6 hours; and removing 3-300 parts by weight of water to obtain viscous liquid; and (2) using the viscous liquid obtained in the step (1) as a partial furfuryl alcohol substitute and preparing the novel modified furan resin for casting according to the conventional process of furan resin for casting, wherein the using amount of the viscous liquid is equivalent to the weight of furfuryl alcohol to be substituted and accounts for 1-20 percent of the total weight of a furan resin synthetic raw material for casting. The method is simple, feasible and environmentally-friendly, and a reticulate structure of the resin is formed during curing, so that the intensity of furan resin sand for casting can be improved.
Description
Technical field
The invention belongs to furan resin for casting synthesis technology field, be specifically related to a kind of preparation method of new modified furan resin for casting.
Background technology
The binder for casting system is comprised of resin and solidifying agent, catalyzer, and a kind of good binder for casting system must possess good chemical stability, lower viscosity; Resin with have long operable time after roughing sand mixes, have good demolding performace after curing; Enough normal temperature and hot strength; And has good collapsibility and the performance such as sand reclamation is easy.Therefore, the selection of casting resin is most important.
The furfuryl alcohol that furane resin refer to have furan nucleus is the synthetic resin of main raw material.The excellent properties such as in the sixties in last century, furane resin just begin for casting industry, and, diffustivity fast with its cold setting speed better, intensity is higher and synthesis technique is simple obtain develop rapidly, are the casting resins of consumption maximum both at home and abroad at present.
As everyone knows, the content of furfuryl alcohol in furan resin for casting is higher, and its cohesive strength is higher, so the cost of resin is subjected to the impact of furfuryl alcohol very large.The step of preparation furfuryl alcohol is more loaded down with trivial details, and adopting the seasonal agricultural byproducts such as corn cob and crop straw is that raw material obtains furfural through hydrolysis, high temperature dehydration cyclisation, and last furfural obtains furfuryl alcohol after shortening again, so the preparation cost of furfuryl alcohol is higher.In addition, the preparation of furfural exist productive rate low, produce the problems such as a large amount of residues, waste gas.Therefore need the suitable furfuryl alcohol substitute of preparation badly for the preparation of furan resin for casting, make it to keep original performance, but and the cost of decrease furan resin for casting and protection of the environment.
Viswanathan T etc. discloses and has added urea to prepare the method for wood adhesive in a kind of carbohydrate, namely add urea in the carbohydrate aqueous solution, after making its thermal dehydration under catalyst action generate 5 hydroxymethyl furfural, form water-soluble or low viscosity emulsus with the urea reaction polymerizable and without polymer resin [the Viswanathan T of precipitation, Richardson T.Thermosetting adhesive resins:US, 4524164[P] .1985-06-18.].This tackiness agent need be heated to comparatively high temps (160～200 ℃) after adding solidifying agent, and (can crosslinked action occur under 300～1000psi) and solidify, set time is very short by (5～15min) at high pressure.Require to compare with the casting technique over-all properties that satisfies of addressing previously, this wood adhesive is not suitable for directly as casting resin.
Therefore, how to utilize the advantage of carbohydrate and urea reaction, a kind of novel high-performance furan resin for casting is provided, the standby raw material sources of this resin are wide, preparation technology is simple, with low cost, this resin contains a large amount of furan nucleuss, the higher furfuryl alcohol of price in can alternative materials has important theory significance and using value.
Summary of the invention
Problem for existing furan resin for casting existence, the object of the invention is to provide a kind of preparation method of new modified furan resin for casting, utilize carbohydrate to obtain for main raw material the resin that contains a large amount of furan nucleuss that a kind of raw material sources are wide, preparation technology is simple, with low cost, be used for substituting the higher furfuryl alcohol of price and prepare furane resin, keeping resinogen to have on the basis of performance, obtaining cheaply, casting resin has important theory significance and using value.
In order to solve these problems of the prior art, technical scheme provided by the invention is:
A kind of preparation method of new modified furan resin for casting is characterized in that said method comprising the steps of:
(1) 100 weight part carbohydrates, 0.1～40 part of urea are dissolved in 30～200 weight parts waters, then add 5～60 weight part acid, after reacting 0.5～10 hour under the temperature condition of 60～105 ℃, add 0.1～40 parts by weight of formaldehyde after after being cooled to 30～90 ℃, the pH value being transferred to 7.5～10, be warming up to 60～100 ℃ of reactions 0.5～6 hour, then remove 3～300 weight parts waters, obtain thick liquid;
(2) thick liquid that step (1) is obtained is as part furfuryl alcohol substitute, is prepared new modified furan resin for casting according to the common process of furan resin for casting; The consumption of described thick liquid is suitable with furfuryl alcohol weight to be substituted, and is 1%～20% of furan resin for casting synthesis material gross weight.
Preferably, the common process of the middle furan resin for casting of described method steps (2) comprises makes formaldehyde, urea (and/or phenol) etc. carry out addition reaction under alkaline condition, then carries out polycondensation with furfuryl alcohol under acidic conditions and obtains.
Preferably, in described method steps (1), 100 weight part carbohydrates, 0.5～40 part of urea are dissolved in 30～200 weight parts waters, then add 5～60 weight part acid, after reacting 0.5～10 hour under the temperature condition of 60～105 ℃, add 0.5～40 parts by weight of formaldehyde after after being cooled to 30～90 ℃, the pH value being transferred to 7.5～10, be warming up to 60～100 ℃ of reactions 0.5～6 hour, then remove 3～300 weight parts waters, obtain thick liquid;
Preferably, in described method steps (1) carbohydrate be selected from five carbon monose, six carbon monose, one or more the arbitrary combination in the disaccharides that consisted of by five carbon, six carbon monose structural units, the polysaccharide that consisted of by five carbon, six carbon monose structural units.
Preferably, acid is selected from hydrochloric acid, nitric acid, sulfuric acid, phosphoric acid, boric acid, acetic acid, oxalic acid, tosic acid, citric acid, succinic acid, tartaric one or more arbitrary combination, described sour water soluble in described method steps (1).
Preferably, the basic solution of adjusting the employing of pH value in described method steps (1) is selected from a kind of alkaline aqueous solution of sodium hydroxide, potassium hydroxide, ammoniacal liquor or two or more arbitrary combination, and the mass percent concentration of basic solution is 10～40%.
The purpose of this invention is to provide a kind of joining take low-cost carbohydrate as main raw material and a small amount of urea and formaldehyde synthetic resins, replace the part furfuryl alcohol to be used for the preparation of new modified furan resin for casting, on the basis that keeps original performance, this furane resin cost obviously reduces.Take water as solvent, adopt carbohydrate and urea, formaldehyde reaction to make thick liquid in preparation method of the present invention, replace furfuryl alcohol for the preparation of new modified furan resin for casting.Contain in new modified furan resin for casting urine aldehyde and or resol, need add furfuryl alcohol allotment at last stage reaction and form.
The concrete preparation method of the present invention comprises:
(1) by weight: 30～200 parts of water, 100 portions of sugar and 0.1～40 part of urea add in reaction vessel, are stirred to dissolving under 50 ℃, then add 5～60 parts of acid, react under the temperature condition of 60～105 ℃ 0.5～10 hour; Thereafter lowering the temperature adds basic solution that PH is transferred to 7.5～10 after 30～90 ℃, adds 0.1～40 part of formaldehyde, and 60～100 ℃ of reactions 0.5～6 hour that heat up remove 5～300 parts of water, obtain a kind of reddish brown or black thick liquid.
(2) reddish brown or black thick liquid product are replaced 1～20 part of furfuryl alcohol, the conventional preparation technology who is used for furane resin, stir, get product, concrete, the thick liquid that step (1) is obtained, then carries out polycondensation with furfuryl alcohol and obtains being prepared the Modified Cast furane resin according to first making formaldehyde, urea carry out addition reaction under alkaline condition as part furfuryl alcohol substitute under acidic conditions; The consumption of described thick liquid is 1%～20% of furan resin for casting synthesis material gross weight.
Preferably, described sugar is six carbon monose, and the disaccharides and the polysaccharide that contain six carbon monose structural units, or is one or more composition wherein.Preferably, acid is selected from hydrochloric acid, nitric acid, sulfuric acid, phosphoric acid, boric acid, acetic acid, oxalic acid, tosic acid, citric acid, succinic acid, tartaric one or more arbitrary combination, described sour water soluble in described method steps (1).Preferably, described method steps (1) neutral and alkali solution is selected from a kind of alkaline aqueous solution of sodium hydroxide, potassium hydroxide, ammoniacal liquor or two or more arbitrary combination, and the mass percent concentration of basic solution is 10～40%.
The new modified furan resin for casting that obtains refer to furane resin contain urine aldehyde and or resol, need add furfuryl alcohol at conventional cast latter stage with the furane resin building-up reactions and allocate and form, adopt 1～20 part of furfuryl alcohol of thick liquid product replacement that obtains during allotment.Thick liquid is as the furfuryl alcohol substitute, and its consumption is suitable with the weight of the furfuryl alcohol that needs to substitute.
The invention provides a kind of preparation method of furan resin for casting, proposed a kind of resin that synthesizes with urea and formaldehyde take low-cost carbohydrate as main raw material, replace the higher furfuryl alcohol of price to be used for the preparation method of furan resin for casting.In method, thick liquid is as the furfuryl alcohol substitute, and its consumption is suitable with the weight of the furfuryl alcohol that needs to substitute.
With respect to scheme of the prior art, advantage of the present invention is:
In preparation method of the present invention, the carbohydrate wide material sources, cheap, and the resin that contains furan nucleus that is synthesized is used for the alternative furfuryl alcohol of part and prepares furan resin for casting, and cost obviously reduces; Because the intermediate product 5 hydroxymethyl furfural has hydroxyl and two active groups of aldehyde radical, compare with furfuryl alcohol, increased the cross-linking set of resin solidification, be conducive to resin and form reticulated structure in solidification process, thereby can improve the intensity of furan resin for casting sand; The present invention has the characteristics of technique simple possible, environmental protection, has good development prospect.
In sum, the invention provides the preparation method that a kind of novel casting is used furane resin.By weight: 30～200 parts of water, 100 portions of sugar and 0.1～40 part of urea are added in reaction vessel, be stirred to dissolving under 10～60 ℃, then add 5～60 parts of acid, reacted under the temperature condition of 60～105 ℃ 0.5～20 hour; Thereafter lowering the temperature adds basic solution that PH is transferred to 7.5～10 after 30～90 ℃, adds 0.1～40 part of formaldehyde, and 60～100 ℃ of reactions 0.5～6 hour that heat up remove 5～300 parts of water, obtain a kind of reddish brown or black thick liquid.Then, with reddish brown or black thick liquid product and urine aldehyde and or resol, and the furfuryl alcohol discharging that stirs namely gets furan resin for casting.In the situation that performance is constant, the furfuryl alcohol that this thick liquid product is alternative 1～20 part.The present invention has that preparation is simple, and reaction conditions is gentle, and the characteristics such as environmental friendliness are convenient to suitability for industrialized production, and gained furane resin stability and transparency good, the 24h room temperature tensile strength is high, material cost significantly reduces.
Embodiment
Below in conjunction with specific embodiment, such scheme is described further.Should be understood that these embodiment are not limited to limit the scope of the invention for explanation the present invention.The implementation condition that adopts in embodiment can be done further adjustment according to the condition of concrete producer, and not marked implementation condition is generally the condition in normal experiment.
Comparative Examples
Routine casting is as follows with the preparation process of furane resin:
(1) 11g water, 6g solid formaldehyde and 10g liquid formaldehyde (37%) are packed in reactor, 80～85 ℃ are stirred and be warmed up in the sodium hydroxide adjust pH to 9 with 30%～9.5, treats that solid is entirely molten;
(2) then be cooled to 40～50 ℃, add urea 9.8g, adjust pH to 8～8.5 are warmed up to 80～85 ℃, insulation reaction 1.5h;
(3) be cooled to 40～50 ℃, add the 20g furfuryl alcohol, with hydrochloric acid (1:3) adjust pH 4～4.5, be warmed up to 90～105 ℃, insulation reaction 100min;
(4) be cooled to 40～50 ℃, with ammonia soln adjust pH to 7～8.5, then add 40g furfuryl alcohol and 0.85g silane coupling agent, stir the 30min discharging, its performance sees Table 1.
Embodiment 1:
30g water, 100g sucrose and 0.1g urea are added in reaction vessel, be stirred to dissolving under 10 ℃, then add the 5g vitriol oil, stir and be warmed up to 60 ℃, reaction 20h cools to 30 ℃; Sodium hydroxide with 30% is transferred pH value to 7.5, adds the formaldehyde of 0.1g, the 60 ℃ of reaction 6h that heat up, and the 5g that dewaters thereafter obtains the red-brown thick liquid.
According to the Comparative Examples corresponding step, under the constant condition in step (1)～(3), get above-mentioned red-brown thick liquid 5g and substitute 5g furfuryl alcohol in comparative example step (4) (raw material gross weight 5%) in step (4), the actual raw material of participating in reaction is 35g furfuryl alcohol, 5g red-brown thick liquid and 0.85g silane coupling agent, the constant Modified Cast furane resin that obtain of other conditions, its performance sees Table 1.
Embodiment 2:
60g water, 100g glucose and 5g urea are added in reaction vessel, be stirred to dissolving under 30 ℃, then add the 10g concentrated nitric acid, stir and be warmed up to 80 ℃, reaction 4h cools to 40 ℃; Sodium hydroxide with 30% is transferred pH value to 8.5, adds the formaldehyde of 6g, the 70 ℃ of reaction 4h that heat up, and the 80g that dewaters thereafter obtains the red-brown thick liquid.
According to the Comparative Examples corresponding step, under the constant condition in step (1)～(3), get above-mentioned red-brown thick liquid 5g and substitute 10g furfuryl alcohol in comparative example step (4) (raw material gross weight 10%) in step (4), the actual raw material of participating in reaction is 30g furfuryl alcohol, 10g red-brown thick liquid and 0.85g silane coupling agent, the constant Modified Cast furane resin that obtain of other conditions, its performance sees Table 1.
Embodiment 3:
76g water, 100g sucrose and 7.5g urea are added in reaction vessel, be stirred to dissolving under 40 ℃, then add the 25g concentrated hydrochloric acid, stir and be warmed up to 84 ℃, reaction 2h cools to 50 ℃; Ammoniacal liquor with 20% is transferred pH value to 8.5, adds the formaldehyde of 8g, the 95 ℃ of reaction 1h that heat up, and the 98g that dewaters thereafter obtains the red-brown thick liquid.
According to the Comparative Examples corresponding step, under the constant condition in step (1)～(3), get above-mentioned red-brown thick liquid 20g and substitute 20g furfuryl alcohol in comparative example step (4) (raw material gross weight 20%) in step (4), the actual raw material of participating in reaction is 20g furfuryl alcohol, 20g red-brown thick liquid and 0.85g silane coupling agent, the constant Modified Cast furane resin that obtain of other conditions, its performance sees Table 1.
Embodiment 4:
100g water, 100g starch and 10g urea are added in reaction vessel, be stirred to dissolving under 35 ℃, then add 15g boric acid, stir and be warmed up to 90 ℃, reaction 3h cools to 40 ℃; Potassium hydroxide with 30% is transferred pH value to 8.5, adds the formaldehyde of 10g, the 85 ℃ of reaction 2h that heat up, and the 130g that dewaters thereafter obtains the brownish black thick liquid.
According to the Comparative Examples corresponding step, under the constant condition in step (1)～(3), get above-mentioned brownish black thick liquid 15g and substitute 15g furfuryl alcohol in comparative example step (4) (raw material gross weight 15%) in step (4), the actual raw material of participating in reaction is 25g furfuryl alcohol, 15g brownish black thick liquid and 0.85g silane coupling agent, the constant Modified Cast furane resin that obtain of other conditions, its performance sees Table 1.
Embodiment 5:
120g water, 100g maltose and 20g urea are added in reaction vessel, be stirred to dissolving under 40 ℃, then add 35g oxalic acid, stir and be warmed up to 90 ℃, reaction 6h cools to 60 ℃; Sodium hydroxide with 30% is transferred pH value to 9.5, adds the formaldehyde of 30g, the 80 ℃ of reaction 2h that heat up, and the 140g that dewaters thereafter obtains the brownish black thick liquid.
According to the Comparative Examples corresponding step, under the constant condition in step (1)～(3), get above-mentioned brownish black thick liquid 5g and substitute 5g furfuryl alcohol in comparative example step (4) (raw material gross weight 5%) in step (4), the actual raw material of participating in reaction is 35g furfuryl alcohol, 5g black thick liquid and 0.85g silane coupling agent, the constant Modified Cast furane resin that obtain of other conditions, its performance sees Table 1.
Embodiment 6:
200g water, 100g starch and 40g urea are added in reaction vessel, be stirred to dissolving under 60 ℃, then add the 50g strong phosphoric acid, stir and be warmed up to 105 ℃, reaction 1h cools to 90 ℃; Sodium hydroxide with 40% is transferred pH value to 10, adds the formaldehyde of 40g, the 100 ℃ of reaction 2h that heat up, and the 300g that dewaters thereafter obtains the brownish black thick liquid.
According to the Comparative Examples corresponding step, under the constant condition in step (1)～(3), get above-mentioned brownish black thick liquid 20g and substitute 20g furfuryl alcohol in comparative example step (4) (raw material gross weight 20%) in step (4), the actual raw material of participating in reaction is 20g furfuryl alcohol, 20g brownish black thick liquid and 0.85g silane coupling agent, the constant Modified Cast furane resin that obtain of other conditions, its performance sees Table 1.
The performance test results of the furan resin for casting that each embodiment of table 1 and Comparative Examples obtain
* adopt the Chinese Foundry of Tongliao City large crop type sand company limited preparation to test with self-hardening furan resin standard JB/T7526-2008 according to casting with standard sand, resin amount is 1% of roughing sand weight, and solidifying agent is tosic acid 70% aqueous solution.
Above-mentioned example only is explanation technical conceive of the present invention and characteristics, and its purpose is to allow the person skilled in the art can understand content of the present invention and implement according to this, can not limit protection scope of the present invention with this.All equivalent transformations that spirit is done according to the present invention or modification are within all should being encompassed in protection scope of the present invention.
Claims (5)
1. the preparation method of a new modified furan resin for casting is characterized in that said method comprising the steps of:
(1) 100 weight part carbohydrates, 0.1～40 part of urea are dissolved in 30～200 weight parts waters, then add 5～60 weight part acid, after reacting 0.5～10 hour under the temperature condition of 60～105 ℃, add 0.1～40 parts by weight of formaldehyde after after being cooled to 30～90 ℃, the pH value being transferred to 7.5～10, be warming up to 60～100 ℃ of reactions 0.5～6 hour, then remove 3～300 weight parts waters, obtain thick liquid;
(2) thick liquid that step (1) is obtained is as part furfuryl alcohol substitute, is prepared new modified furan resin for casting according to the common process of furan resin for casting; The consumption of described thick liquid is suitable with furfuryl alcohol weight to be substituted, and is 1%～20% of furan resin for casting synthesis material gross weight.
2. preparation method according to claim 1, it is characterized in that the common process of furan resin for casting comprises in described method steps (2) makes formaldehyde, urea carry out addition reaction under alkaline condition, then carries out polycondensation with furfuryl alcohol under acidic conditions and obtains.
3. preparation method according to claim 1, the arbitrary combination of one or more in the polysaccharide that it is characterized in that disaccharides that carbohydrate in described method steps (1) is selected from five carbon monose, six carbon monose, is made of five carbon, six carbon monose structural units, is consisted of by five carbon, six carbon monose structural units.
4. preparation method according to claim 1, it is characterized in that acid in described method steps (1) is selected from hydrochloric acid, nitric acid, sulfuric acid, phosphoric acid, boric acid, acetic acid, oxalic acid, tosic acid, citric acid, succinic acid, tartaric one or more arbitrary combination, described sour water soluble.
5. preparation method according to claim 1, it is characterized in that the basic solution of adjusting the employing of pH value in described method steps (1) is selected from a kind of alkaline aqueous solution of sodium hydroxide, potassium hydroxide, ammoniacal liquor or two or more arbitrary combination, the mass percent concentration of basic solution is 10～40%.
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| CN105108032A (en) * | 2015-08-11 | 2015-12-02 | 安徽省胜峰机械有限公司 | High-plasticity modified furan resin sand for steel casting and preparation method of high-plasticity modified furan resin sand |
| CN105108046A (en) * | 2015-08-11 | 2015-12-02 | 安徽省胜峰机械有限公司 | High-strength calcium sulphate whisker modified furan resin sand for steel castings and preparation method thereof |
| CN105108044A (en) * | 2015-08-11 | 2015-12-02 | 安徽省胜峰机械有限公司 | Aluminum-magnesium-silicate-contained modified furan resin sand for steel casting and preparing method for aluminum-magnesium-silicate-contained modified furan resin sand |
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| CN105081197A (en) * | 2015-08-14 | 2015-11-25 | 郭伟 | Modified furan resin sand containing nano-mesoporous alumina and used for steel castings and preparation method thereof |
| CN105081198A (en) * | 2015-08-14 | 2015-11-25 | 郭伟 | Modified furan resin sand with sodium bentonite for casting steel and preparation method of modified furan resin sand |
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| CN111185574A (en) * | 2020-03-13 | 2020-05-22 | 浙江浦江精宇铸造有限公司 | Lost foam casting process of nodular iron casting |
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