CN1161415C - Amino resin compositions for cleaning mould - Google Patents
Amino resin compositions for cleaning mould Download PDFInfo
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- CN1161415C CN1161415C CNB001299964A CN00129996A CN1161415C CN 1161415 C CN1161415 C CN 1161415C CN B001299964 A CNB001299964 A CN B001299964A CN 00129996 A CN00129996 A CN 00129996A CN 1161415 C CN1161415 C CN 1161415C
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Abstract
The present invention relates to an amino resin composition for cleaning moulds, which has the structure that amino resinoid of a damp dry object type made in a special method is additionally added in general thermosetting resin, in this way, the viscosity of the amino resin composition which is obtained is reduced, and the ingot striking performance of a powder body is improved. When the present invention is used for cleaning the dirt of the surfaces of the moulds, the present invention has good forming ability and mould cleaning effect. The present invention can effectively shorten the time for cleaning the moulds, and because the present invention has the good performance of easy preforming, the problem that the composition of the powder body is tableted uncomfortably can be solved.
Description
Technical field
The present invention relates to the amino resin compositions that a kind of cleaning mold is used.Particularly when moulding, have good imitating clearly really, thereby can reduce clear mould number of times and time saving cost, also have the amino resin compositions for cleaning mould of beating the good characteristic of ingot easily simultaneously.
Background technology
When aspects such as semiconductor device (for example: unicircuit (IC), large-scale unicircuit (LSIC), electric crystal and diode) and electronic circuit are used as curable resins such as Resins, epoxy to packaged material, after the long-time continuous moulding, easily there is material residual; Or certain interval of time if still carry out moulding without cleaning, the contaminated situation in sealing moulding thing surface often takes place, or the sealing moulding thing is attached to the situation that causes sticking to mould on the mould and can't carries out production operation smoothly when moulding and mould inside are not subjected to polluting.Therefore the regular cleaning of mould is rather important, and usually behind hundreds of operations for forming, the resin that should use cleaning mold to use comes cleaning mold guaranteeing the clean of die surface, thereby operations for forming can be carried out smoothly.
Known cleaning mold resin combination, be amino resin compositions, it belongs to thermosetting resin, when device is used in the encapsulation that is used for cleaning semi-conductor or IC part etc., often be made into the ingot sheet earlier before transfer formation, thereby make its energy filling entire die inside, the ingot sheet often need be preheated to 80～120 ℃, treat together to take out together with the dirt of die surface after its forming and hardening is full of entire die, to reach the purpose on cleaning mold surface.
Because the requirement of highly integrated, thin typeization such as IC, LSIC, the real dressization in surface and the unmanned equal altitudes automatization of moulding, automatic molder is widely used, therefore need use the ingot sheet of various different sizes at various devices, its size is generally diameter 10～70mm.Traditional cleaning mold with resin when the ingot panel forming machine carries out the ingot sheet, often cause the mould consume, thereby need use the supersteel material, when so not only having increased cost and from preforming press, having taken out the ingot sheet, cause noise pollution because of the dry and astringent viscous in surface often has attrition accentuated, or easily shortcoming such as break, isolate and cause disqualification rate to improve because of the system ingot is not good.
For example, disclose in the Japanese Patent Publication 64-10162 communique a kind of with amino resin and phenolic resin the cocondensation resin and the cleaning mold resin combination that mineral powder was constituted of new Mohs' hardness 6～15.And also once disclosed a kind of in the public clear 52-788 communique of spy is that material of main part carries out moulding cleaning the method for contaminated die surface with the amino resin, and discloses a kind of by cleaning mold resin that amino resin compositions, organic substrate or inorganic substrate and off-shape agent constituted simultaneously.But in Japanese Patent Publication 52-788 communique, for improving the not good shortcoming of its system ingot to improve qualification rate, increased the content of cleaning mold with lubricant in the resin combination, though can improve qualification rate, but ooze out the phenomenon that pollutes because of lubricant itself has taken place on the contrary in the lubricant content raising, caused the reduction of cleaning mold effect, thereby the ejaculation number (cleaning number of times) when having to increase cleaning mold makes the whole structure variation.The TaiWan, China patent also discloses a kind of amino resin compositions of small-sized ingot sheet form for No. 343171, but its curing speed is too fast, cause the ability on cleaning mold surface to reduce, thus the ejaculation number must increase cleaning mold the time, thus increased mold cleaning cost and required time.In view of this, the range of choice that people wish to develop a kind of condition of molding always is wide, and it is good to play ingot, easily ingot sheetization and have the resin combination of good cleaning.
For this reason, the purpose of this invention is to provide a kind of amino resin compositions for cleaning mould, it has good forming ability when being used for cleaning mold surface dirt, have good imitating clearly really, can effectively shorten the clear mould time, and because of it has the good characteristic of easy system ingot, so can solve the problem that powder composition is difficult for ingotization.
For achieving the above object, the inventor discovers the amino resin that adds in right amount the half-dried thing form that makes with ad hoc approach in general thermosetting resin, for example, can increase the consistency of resin during trimeric cyanamide-phenol-formaldehyde cocondensation compound, reduce the viscosity of resin combination powder and the thermostability of raising resin, increase the clear mould ability of resin combination, and so the resin combination apparent density of gained improves, even after adding lubricant, also can keep good cleaning mold, improved the production qualification rate of ingot tablet simultaneously widely.
Summary of the invention
Amino resin compositions for cleaning mould of the present invention, said composition comprise the thermosetting resin of 30～60wt% and the amino resin that contains at least one methylol of 40～70wt%, and its solid form component content is 75wt% at least.
Particularly, the invention provides a kind of amino resin compositions for cleaning mould, said composition comprises the thermosetting resin of 40～50wt% and the half-dried thing form amino resin that contains at least one methylol of 20～30wt%, and the solid form component content of this half-dried thing form amino resin is 75～85wt%, and wherein this thermosetting resin is melamine resin and derivative thereof; This amino resin is by the aminocompound or derivatives thereof, and the formaldehyde or derivatives thereof reacts and make, or by aminocompound or derivatives thereof, formaldehyde or derivatives thereof, and the phenol or derivatives thereof reacts and makes.
In amino resin compositions for cleaning mould of the present invention, also can further comprise lignocellulosic material, mineral filler, lubricant, curing catalyst.It is the amino resin that adds in addition a kind of half-dried thing form that makes with ad hoc approach in general thermosetting resin, and this mixture ground jointly with lignocellulosic material, mineral filler, lubricant, promotor again and uniform mixing and.So the composition of gained can directly be played ingot and make the ingot sheet, no matter make the big ingot sheet form that needs first preheating to re-use, the small-sized ingot sheet form that does not still need preheating to use, its system ingot is all superior, production qualification rate height, the ingot sheet that makes also has very good cleaning to mould.
Amino resin used in the present invention is meant general amino resin such as melamine resin etc.
The amino resin of the half-dried thing form that makes with ad hoc approach used in the present invention is the aminoresin that contains at least one methylol, and the example is for example melamine formaldehyde resin, trimeric cyanamide-resinox and melamine-urea-formaldehyde resin, urea-formaldehyde resin etc.The manufacture method of the amino resin of this half-dried thing form is with aminocompound or derivatives thereof such as urea, trimeric cyanamide and formaldehyde or derivatives thereof and the phenol or derivatives thereof that adds according to circumstances, there is down the aminoresin of the half-dried thing forms of making through the reflux stirring such as urea-formaldehyde resin, urea-resinox, melamine formaldehyde resin or trimeric cyanamide-resinox in catalyzer.Need to be controlled at the F/M molar ratio of formaldehyde or formaldehyde derivatives (hereinafter representing with F) and aminocompound (hereinafter representing with M) be more than 1.0 to the ratio of aminocompound PARA FORMALDEHYDE PRILLS(91,95) and derivative thereof in this reaction, makes the formaldehyde (F) that can be used as linking agent in the resin could produce crosslinking curing more than urea or trimeric cyanamide (M).The F/M of reaction can be 1.0～6.0, is preferably 1.0～2.5.If under the situation that contains the phenol or derivatives thereof, the total mole number (P+F) of phenol or derivatives thereof and formaldehyde or formaldehyde derivatives is 1.0～6.0 to the ratio ((P+F)/(M)) of the mole number (M) of aminocompound, is preferably 1.0～2.5.
Catalyst system therefor can be the oxide compound of alkaline-earth metal of the basic metal of I main group in the periodictable for example and II main group or alkaline matter of oxyhydroxide or ammonia soln and other amines etc.Above-mentioned catalyzer can separately or merge use more than two kinds, its addition is to be advisable than≤5% to the reactant gross weight.
Temperature of reaction can be 50～100 ℃, this reaction process has mainly obtained the amino resin of half-dried thing form, so drying under reduced pressure is with stopped reaction when the gelation time of reactant makes it, and adjust degree of drying with the control moisture content according to the content of required solid form composition, the content of solid form composition is reached more than 75% is advisable, preferably reach more than 85%, promptly make the amino resin of the half-dried thing form that contains at least one methylol, its degree of dehydration is controlled at and makes the solid form composition reach 75% or higher.Gelation time is measured according to the method for JIS K6909, can the stringy time for being stirred on hot plate.
This processing procedure and conventional dry method are compared, the present invention does not use the solid amino resin of high price, also other interpolation solvent as damp process not, thereby can omit the dry step of removing solvent, and can be owing to organic solvent volatilization and contaminate environment when dry, and reduced cost, real is a kind of good processing procedure.
Amino resin compositions for cleaning mould of the present invention comprises: will cooperate other thermosetting resins and other additives in the partial desiccation mode with the amino resin that contains at least one methylol of the half-dried thing form of aforesaid method gained, at for example kneader, ball mill, rotary drum, after evenly mixing in the whipping devices such as positive mixer, add cylinder machine or list, mixing in the twin screw extruder, after making the amino resin of half-dried thing form crosslinked, be broken into particulate state or powdery with the test portion cooling and with pulverizer, thereby obtained the amino resin compositions that cleaning mold of the present invention is used.
Described other additives can be for example paper, wood powder fibrous material, mineral filler, lubricant, curing catalyst etc.
The preparation method of amino resin compositions for cleaning mould of the present invention, its be use separately the solid form composition be higher than 75% and contain at least a methylol half-dried thing form amino resin or with other thermosetting resins and use, under the partial desiccation state, aggregate into the amino resin formed material of larger molecular weight with the amino resin of other additives through adding the hot milling step and making half-dried thing form, this material is amino resin compositions for cleaning mould of the present invention.Method of the present invention has merged the advantage of conventional dry, wet method and its shortcoming of having forgone, the drying step that can omit damp process also can be avoided the solvent evaporates of a large amount of hypertoxicities, stink, the transferring cleaning problem that need not use the expensive raw material in the dry type method for making and avoid the powder thing to cause simultaneously.Simple and the use that can omit organic solvent of recipe step of the present invention, and the phenomenon of having avoided powder to fly upward, thus utility value in economy and the environmental protection had.
The addition of employed general thermosetting resin is about 30～60wt% of amino resin compositions total amount among the present invention, is preferably about 40～50wt%.
The amino resin of employed half-dried thing form among the present invention, its addition are about about 20～30wt% of amino resin compositions total amount.
Paper pulp used in the present invention, wood powder fibrous material, its Fibre diameter and size are good with the particle (being the particle of particle diameter less than 0.17mm) that can sieve by 80# that contains more than the 80wt%, contain the above person of 95wt% for better.The adding proportion of paper pulp, wood powder fibrous material is 8～10wt% of amino resin composition total amount.
Mineral filler used in the present invention comprises metallic compound such as silicon, iron, titanium, sodium, calcium, chromium, manganese, boron, the compound of aluminium etc., for example metal oxide or oxyhydroxide are (for example: magnesium oxide, calcium oxide, zinc oxide, manganese oxide, aluminum oxide, silicon oxide, silicon-dioxide, aluminium hydroxide, magnesium hydroxide etc.), metal carbonate, metal sulfate and sulfide are (for example: calcium sulfate, barium sulfate, zinc sulphide etc.), metal silicate (for example: Magnesium Silicate q-agent, Calucium Silicate powder etc.), carbide (for example: silicon carbide etc.), the mineral substance powder (for example: silicon carbide, lapis amiridis, talcum powder, diatomite, kaolin, talcum powder, silica, cerasite etc.), or glass fibre (glass fibre length L is below the L/D=5000 to the ratio of glass fiber diameter D) etc., the adding proportion of mineral filler is 0.01～80wt% of amino resin composition total amount, is preferably 10～20wt%.
Employed mineral substance powder can comprise for example natural mineral stones such as silicon carbide, lapis amiridis, talcum powder, diatomite, kaolin, silica, cerasite in the above-mentioned mineral filler, and the oxide compound of silicon, iron, titanium, sodium, calcium, chromium, manganese, boron, aluminium etc. or carbide etc., the diameter of particle size is then to be advisable below the median size 150 μ m, be preferably below the 100 μ m, and median size most preferably is below the 40 μ m.The especially preferred median size of mineral filler is less than the silica flour of 20 μ m.
Lubricant used in the present invention comprises that the fats lubricant (for example: stearic acid, Zinic stearas, Magnesium Stearate, calcium stearate, butyl stearate etc.), the fatty amide series lubricant agent (for example: the dodecane acid amides, myristamide, oleylamide, the lubricant of saturated or unsaturated monoamide type such as stearylamide and two oleylamide, the lubricant of saturated or unsaturated bisamide type such as bis-stearamides), the alcohol series lubricant agent (for example: poly(oxyethylene glycol) 400 (PEG400), PEG1000, higher alcohols etc.), the paraffin class lubricant (is mainly the straight chain type hydrocarbon polymer that contains 28～90 carbon, for example: liquid wax, paraffin, petroleum wax (ParaffinWax), Sa alcohol wax (Sasol Wax) etc.) and siliceous lubricant (for example: silicone oil etc.).The addition of lubricant is 0.01～10wt% in the amino resin compositions total amount, is preferably 1.5～5.0wt%.When for example being fatty acid metal salt (as Zinic stearas, Magnesium Stearate, calcium stearate), it can be 1.5～10wt%, and when being lipid acid (as hard fat acid, butyl stearate), then it can be 0.01～0.1wt%, qualification rate and throughput rate when improving the lozenge moulding, and guarantee its stability and grab the effect of dirt, clear mould.When if above-mentioned lubricant addition is not enough, amino resin compositions can not be full of the complicated small part in the mould structure, thereby cause cleaning poor effect, and amino resin compositions is attached to die surface after solidifying because of separability is not good, has therefore caused clear mould insufficient.
The curing catalyst that curing catalyst used in the present invention comprises inorganic acids (for example: sulfuric acid, boric acid, phosphoric acid, hydrochloric acid etc.), the curing catalyst of organic acid (for example: oxalic acid, phenylformic acid, anhydride phthalic acid, right-toluenesulphonic acids etc.), organic amine salt curing catalyst (aforementioned acids and trolamine, triethylamine, the salt that the 2-methyl-2-amino-1-propyl alcohol etc. is formed, for example: Japanese Ri Dongli grinds the organic amine salt curing catalyst CATANITTO that Industrial Co., Ltd sells, CATANITTO-A etc.), inorganic metal salt curing catalyst (for example: zinc sulfite etc.) or the like, the addition of curing catalyst is 0.01～0.4wt% of amino resin compositions total amount.
Amino resin compositions for cleaning mould of the present invention can be made into ingot sheet, en plaque or powder shaped, thereby has good imitating clearly really.
The present invention will be described in more detail below in conjunction with embodiment and comparative example, but be not to be used to limit the scope of the invention.
Gelation time among above-mentioned specification sheets and the embodiment is can the stringy time (measuring down in 150 ℃) according to being stirred on hot plate of the method mensuration of JIS K6909.
The curing speed of amino resin compositions for cleaning mould of the present invention (T90 value) is 450～750 seconds, and this curing speed is measured as follows:
The measuring method of curing speed (T90 value)
Use commercially available JSR type maturation meter (curemeter), when mold surface temperature maintains 145 ℃, add that the vibration of certain amplitude makes it distortion,, detect the situation that cleaning mold takes place with the resin combination STRESS VARIATION with passing set time.When STRESS VARIATION reach maximum 90% the time, the needed time is T90 value (second).
Embodiment
Embodiment 1
Trimeric cyanamide 310 weight parts, phenol 130 weight parts, 37% formalin 540 weight parts and calcium hydroxide 5 weight parts are packed in the flask, in 80 ℃ of following backflow reacting by heating after 30 minutes, be cooled to 45 ℃, again in 85 ℃ of following backflow reacting by heating 60 minutes and in 10% sodium hydroxide and after, through drying under reduced pressure, obtain solid form composition 85%, the amino resin of the half-dried thing form of trimeric cyanamide-P-F of gelation time 4 minutes 30 seconds (measuring down) in 150 ℃.
In resin combination total amount 100wt%, get aminoresin 20wt%, melamine resin 50wt%, following silica flour 20wt%, Zinic stearas 1.82wt%, PEG400 0.08wt%, paper pulp 8wt% and the phenylformic acid 0.1wt% of mean particle size 20 μ m of this half-dried thing form, with sphere grinder they are evenly pulverized mixing, or also can use other moiety evenly can be pulverized and well-mixed method, thereby obtain the amino resin compositions that cleaning mold is used.
Embodiment 2
In resin combination total amount 100wt%, after getting the trimeric cyanamide-P-F amino resin 25wt% and paper pulp 10wt% combination drying of the half-dried thing form among the embodiment 1, add again after melamine resin 45.7wt%, mean particle size 20 μ m following silica flour 17wt%, Zinic stearas 1.8wt%, phenylformic acid 0.2wt% and CATINITTO 0.2wt% evenly pulverize mixing with sphere grinder, add PEG400 0.1wt% again and carry out the latter end mixing, obtain the amino resin compositions that cleaning mold is used.
Embodiment 3
Formalin 550 weight parts of trimeric cyanamide 340 weight parts, urea 100 weight parts and 37% are packed in the flask, in 70 ℃ of following backflow reacting by heating after 50 minutes, be cooled to 50 ℃, again in 100 ℃ of following reflux 100 minutes and drying under reduced pressure, obtain solid form composition 85%, the amino resin of the half-dried thing form of trimeric cyanamide-urea-formaldehyde of gelation time 5～6 minutes (measuring down for 150 ℃).
In resin combination total amount 100wt%, get aminoresin thing 30wt%, melamine resin 48wt%, following silica flour 20wt%, Zinic stearas 1.8wt%, PEG400 0.08wt% and the phenylformic acid 0.12wt% of mean particle size 20 μ m of this half-dried thing form, with sphere grinder they are evenly pulverized mixing, or also can use other moiety evenly can be pulverized and well-mixed method, thereby obtain the amino resin compositions that cleaning mold is used.
Embodiment 4
Except that the phenylformic acid among the embodiment 1 is reduced to the 0.01wt% by 0.1wt%, all the other are all operated according to the same procedure of embodiment 1, to obtain the amino resin compositions that cleaning mold is used.
Embodiment 5
Remove and change the half-dried thing among the embodiment 11 into 30wt% by 20wt%, melamine resin is changed into outside the 40wt% by 50wt%, and all the other are all operated according to the same procedure of embodiment 1, to obtain the amino resin compositions that cleaning mold is used.
Comparative example 1
Remove lubricant stearic acid zinc and PEG400 (polyoxyethylene glycol) among the embodiment 1, silica flour changes into beyond the 21.8wt%, and all the other are all operated according to the same procedure of embodiment 1, to obtain the amino resin compositions that cleaning mold is used.
Comparative example 2
Only remove the lubricant stearic acid zinc among the embodiment 1, all the other are all operated according to the same procedure of embodiment 1, to obtain the amino resin compositions that cleaning mold is used.
Comparative example 3
Only remove the lubricant PEG 400 among the embodiment 1, silica flour changes into beyond the 20.08wt%, and all the other are all operated according to the same procedure of embodiment 1, to obtain the amino resin compositions that cleaning mold is used.
Comparative example 4
Remove the lubricant stearic acid zinc among the embodiment 1 is increased to 11.72wt%, and silica flour changes 15wt% into, melamine resin changes into beyond the 15wt%, all the other are all operated according to the same procedure of embodiment 1, to obtain the amino resin compositions that cleaning mold is used.
Comparative example 5
Change into the 21wt% except that the lubricant stearic acid zinc among the embodiment 1 being changed into 0.72wt% and silica flour, all the other are all operated according to the same procedure of embodiment 1, to obtain the amino resin compositions that cleaning mold is used.
Comparative example 6
Remove the aminoresin of the half-dried thing form among the embodiment 2 is reduced to 10wt% by 20wt%, melamine resin is increased to outside the 59wt% by 49wt%, and all the other are all operated according to the same procedure of embodiment 2, to obtain the amino resin compositions that cleaning mold is used.
Comparative example 7
The amount that changes 1.2wt% and PEG400 except that the amount with Zinic stearas among the embodiment 2 into changes into the 0.6wt%, and all the other are all operated according to the same procedure of embodiment 1, to obtain the amino resin compositions that cleaning mold is used.
With the resin combination that the cleaning mold of above embodiment and comparative example is used, carry out following each test with performance that compares its cleaning mold and the quality of making ingot.
The scale removal test of test method 1 die surface
Commercially available epoxy resin molding material ingot sheet, for example SUMIKON 7320CR through behind sealing moulding product 1000 moulds, can make die surface be polluted in the mould of automatic molder, and needs to use amino resin compositions for cleaning mould to clean.Relation between ejaculation number of times of cleaning usefulness (that is cleaning number of times) and cleaning effect is assessed with following method.In this test method, the die temperature during moulding is 180 ℃, and be 180 seconds set time.Its evaluation criteria is as follows:
5: it is residual not have dirt fully
4: it is residual almost not have dirt
3: have dirt residual slightly
2: have dirt residual
1: a lot of dirts are residual
Test example 1
The amino resin compositions that use is used according to the cleaning mold that method obtained of the various embodiments described above and comparative example, carry out the scale removal test on cleaning mold surface and judge the cleaning effect according to the evaluation criteria of test method 1 with test method 1, its result is as shown in table 1.Can confirm fully that by table 1 amino resin compositions that cleaning mold of the present invention is used has extremely excellent imitating clearly really, after penetrating 2 to 3 moulds, promptly removed the dirt of die surface fully, reach standards of grading " 5 ", be much better than comparative example and need penetrate 8 to 9 moulds and can obtain effect same.
The scale removal test of table 1 die surface
| Resin combination | * the cleaning mold of resin combination | |||||||||
| Clear mould number of times | ||||||||||
| 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 | |
| Embodiment 1 | 3 | 5 | - | - | - | - | - | - | - | - |
| Embodiment 2 | 3 | 5 | 5 | - | - | - | - | - | - | - |
| Embodiment 3 | 3 | 4 | 5 | - | - | - | - | - | - | - |
| Embodiment 4 | 3 | 4 | 5 | - | - | - | - | - | - | - |
| Embodiment 5 | 3 | 4 | 5 | - | - | - | - | - | - | - |
| Comparative example 1 | 3 | 2 | 2 | 3 | 3 | 4 | 4 | 4 | 5 | - |
| Comparative example 2 | 1 | 1 | 2 | 2 | 2 | 3 | 4 | 4 | 5 | - |
| Comparative example 3 | 1 | 2 | 3 | 3 | 3 | 4 | 4 | 4 | 5 | - |
| Comparative example 4 | 1 | 2 | 2 | 3 | 3 | 4 | 4 | 5 | - | - |
| Comparative example 5 | 2 | 2 | 2 | 3 | 3 | 4 | 4 | 5 | - | - |
| Comparative example 6 | 2 | 2 | 2 | 3 | 3 | 4 | 4 | 4 | 5 | - |
| Comparative example 7 | 2 | 2 | 2 | 3 | 3 | 4 | 4 | 4 | 5 | - |
*: its appraisal procedure is as described in the test method 1.
Imitating clearly really of test method 2 different mold temperatures and set time
Commercially available epoxy resin molding material ingot sheet, for example SUMIKON 5050S through behind sealing moulding goods 500 moulds, can make die surface be polluted in the mould of automatic molder, and the amino resin compositions that needs to use cleaning mold to use cleans.In this test method, the die temperature during respectively with moulding is 150 ℃, 160 ℃, 170 ℃, 180 ℃, 190 ℃, and be 180 seconds, 240 seconds, 300 seconds set time, and each penetrates 3 moulds and carries out 3 cleanings, judges the cleaning effect according to the evaluation criteria of test method 1.
Test example 2
Use is according to the amino resin compositions for cleaning mould that method obtained of the various embodiments described above and comparative example, the mould of differing temps and difference are under set time during respectively at moulding, carry out the scale removal test on cleaning mold surface, each penetrates 3 moulds and cleans, judge the cleaning effect according to the evaluation criteria of test method 2, its result is as shown in table 2.Can confirm fully that by table 2 amino resin compositions for cleaning mould of the present invention has extremely excellent imitating clearly really.Composition of the present invention solidifies and can obtain complete descale effect in 180 seconds or 240 seconds under the low forming mould temperature of 150 ℃ or 160 ℃, need not higher temperature and reaches longer set time.Even and comparative example still can't obtain the effect of complete scale removal under the longer set time of the comparatively high temps of 170 ℃ and 180 ℃ and 300 seconds, and only when using 190 ℃ high temperature and long 300 seconds set times, can obtain effect same.The fruit of imitating clearly that proves the present composition thus is much better than comparative example.
Different die temperatures of table 2 and the scale removal of set time test
| The experimental project explanation | The cleaning of resin combination | |||||
| Resin combination | 150℃ | 160℃ | 170℃ | 180℃ | 190℃ | |
| Embodiment 1 | 180 seconds | 4 | 4 | 5 | 5 | 5 |
| 240 seconds | 4 | 5 | 5 | 5 | 5 | |
| 300 seconds | 5 | 5 | 5 | 5 | 5 | |
| Embodiment 2 | 180 seconds | 4 | 4 | 5 | 5 | 5 |
| 240 seconds | 4 | 5 | 5 | 5 | 5 | |
| 300 seconds | 5 | 5 | 5 | 5 | 5 | |
| Embodiment 3 | 180 seconds | 4 | 4 | 5 | 5 | 5 |
| 240 seconds | 4 | 5 | 5 | 5 | 5 | |
| 300 seconds | 5 | 5 | 5 | 5 | 5 | |
| Embodiment 4 | 180 seconds | 4 | 4 | 5 | 5 | 5 |
| 240 seconds | 4 | 5 | 5 | 5 | 5 | |
| 300 seconds | 5 | 5 | 5 | 5 | 5 | |
| Embodiment 5 | 180 seconds | 4 | 4 | 5 | 5 | 5 |
| 240 seconds | 4 | 5 | 5 | 5 | 5 | |
| 300 seconds | 5 | 5 | 5 | 5 | 5 | |
| Comparative example 1 | 180 seconds | 2 | 2 | 2 | 2 | 3 |
| 240 seconds | 2 | 2 | 2 | 3 | 4 | |
| 300 seconds | 3 | 3 | 4 | 4 | 5 | |
| Comparative example 2 | 180 seconds | 2 | 2 | 2 | 2 | 3 |
| 240 seconds | 2 | 2 | 3 | 3 | 3 | |
| 300 seconds | 3 | 3 | 4 | 4 | 4 | |
| Comparative example 3 | 180 seconds | 2 | 2 | 2 | 2 | 3 |
| 240 seconds | 2 | 2 | 3 | 3 | 4 | |
| 300 seconds | 3 | 3 | 4 | 4 | 4 | |
| Comparative example 4 | 180 seconds | 2 | 2 | 2 | 2 | 3 |
| 240 seconds | 2 | 2 | 3 | 3 | 4 | |
| 300 seconds | 3 | 3 | 3 | 4 | 5 | |
| Comparative example 5 | 180 seconds | 2 | 2 | 2 | 2 | 3 |
| 240 seconds | 2 | 2 | 3 | 4 | 4 | |
| 300 seconds | 3 | 3 | 4 | 4 | 5 | |
| Comparative example 6 | 180 seconds | 2 | 2 | 2 | 2 | 3 |
| 240 seconds | 2 | 2 | 3 | 3 | 4 | |
| 300 seconds | 2 | 3 | 4 | 4 | 5 | |
| Comparative example 7 | 180 seconds | 2 | 2 | 2 | 3 | 3 |
| 240 seconds | 2 | 2 | 3 | 4 | 4 | |
| 300 seconds | 3 | 3 | 4 | 4 | 5 | |
The system ingot of the amino resin compositions that cleaning mold of the present invention is used is assessed by following method.
The measuring method of test method 3 system ingots
4.5 gram ingot sheet molding resin compositions are fills up to (180mm ψ * 30mmH), be forced into 350Kg/cm in the mould
2And kept 5～20 seconds, slough the patrix repressurize and remove the ingot sheet, calculate and produce 100 ingot sheet required times in the hope of throughput rate, and the outward appearance of gained ingot sheet whether complete (have or not isolate or damaged) in the observation processing procedure, calculate disqualification rate by its number of non-compliances, to assess the system ingot of this resin combination.
The weight of each ingot sheet of weighing gained is in addition further assessed the system ingot of this resin combination to know the weight distribution situation.Evaluation criteria is as follows.
◎: weight error ± 0.1 gram
Zero: weight error ± 0.5 gram
*: weight error ± 1.0 grams
Test example 3
Use is according to the amino resin compositions for cleaning mould that method obtained of the various embodiments described above and comparative example, and according to its system ingot of test method 3 assessments, the result is as shown in table 3.Can confirm fully that by table 3 amino resin compositions for cleaning mould of the present invention has extremely excellent system ingot.Amino resin compositions for cleaning mould of the present invention its throughput rate per minute when playing ingot can reach 420～480, and disqualification rate is extremely low only to be 0～1%, and also extremely even its difference of weight distribution is less than 0.1 gram.Comparative example then when playing ingot its throughput rate per minute only be 60～180, disqualification rate is then up to 12～18%, also inhomogeneous its difference of weight distribution is all greater than 0.5 gram, even greater than 1 gram.The result can confirm that the system ingot of amino resin compositions for cleaning mould of the present invention is much better than comparative example thus.
The system ingot of table 3 amino resin compositions for cleaning mould of the present invention
| The experimental project explanation | The system ingot of resin combination | ||
| Resin combination | Throughput rate (per minute system number of spindles) | Disqualification rate * % | Weight distribution |
| Embodiment 1 | 480 | 0 | ◎ |
| Embodiment 2 | 480 | 0 | ◎ |
| Embodiment 3 | 420 | 1 | ◎ |
| Embodiment 4 | 480 | 1 | ◎ |
| Embodiment 5 | 420 | 0 | ◎ |
| Comparative example 1 | 180 | 12 | ○ |
| Comparative example 2 | 180 | 13 | ○ |
| Comparative example 3 | 60 | 17 | × |
| Comparative example 4 | 120 | 16 | × |
| Comparative example 5 | 60 | 18 | × |
| Comparative example 6 | 120 | 15 | × |
| Comparative example 7 | 120 | 14 | ○ |
* disqualification rate (%)=(damaged number of lozenges/per minute system number of spindles) * 100%
Claims (13)
1. amino resin compositions for cleaning mould, said composition comprises the thermosetting resin of 40～50wt% and the half-dried thing form amino resin that contains at least one methylol of 20～30wt%, and the solid form component content of this half-dried thing form amino resin is 75～85wt%, and wherein this thermosetting resin is melamine resin and derivative thereof; This amino resin is by the aminocompound or derivatives thereof, and the formaldehyde or derivatives thereof reacts and make, or by aminocompound or derivatives thereof, formaldehyde or derivatives thereof, and the phenol or derivatives thereof reacts and makes.
2. amino resin compositions for cleaning mould as claimed in claim 1, wherein said amino resin is selected from melamine formaldehyde resin, trimeric cyanamide-resinox, melamine-urea-formaldehyde resin and urea-formaldehyde resin.
3. amino resin compositions for cleaning mould as claimed in claim 1, it further comprises lignocellulosic material, mineral filler, lubricant, curing catalyst.
4. amino resin compositions for cleaning mould as claimed in claim 3, wherein said mineral filler is selected from metal oxide and oxyhydroxide, metal carbonate, metal sulfate or sulfide, metal silicate and carbide thereof, mineral substance powder and glass fibre, and addition is 10～20wt% of amino resin compositions for cleaning mould weight.
5. amino resin compositions for cleaning mould as claimed in claim 4, wherein said mineral filler are the silica flour of median size less than 20 μ m.
6. amino resin compositions for cleaning mould as claimed in claim 3, wherein said lubricant are fats lubricant, fatty amide series lubricant agent, pure series lubricant agent, paraffin class lubricant and siliceous lubricant.
7. amino resin compositions for cleaning mould as claimed in claim 6, wherein said lubricant are fatty acid metal salt, and addition is 1.5～10wt% of amino resin composition gross weight.
8. amino resin compositions for cleaning mould as claimed in claim 6, wherein said lubricant are lipid acid, and addition is 0.01～0.1wt% of amino resin compositions gross weight.
9. amino resin compositions for cleaning mould as claimed in claim 3, wherein said curing catalyst is inorganic acids curing catalyst, organic acid curing catalyst, organic amine salt curing catalyst, inorganic metal salt curing catalyst, and its adding proportion is 0.01～0.4wt% of amino resin weight.
10. amino resin compositions for cleaning mould as claimed in claim 3, wherein said lignocellulosic material are to contain the particle of the above particle diameter of 80wt% less than 0.17mm, and its addition is 8～10wt% of amino resin compositions total amount.
11. amino resin compositions for cleaning mould as claimed in claim 1, wherein said composition is made into the ingot sheet.
12. amino resin compositions for cleaning mould as claimed in claim 1, wherein said composition is made into en plaque.
13. amino resin compositions for cleaning mould as claimed in claim 1, wherein said composition is made into powder shaped.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB001299964A CN1161415C (en) | 2000-10-30 | 2000-10-30 | Amino resin compositions for cleaning mould |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB001299964A CN1161415C (en) | 2000-10-30 | 2000-10-30 | Amino resin compositions for cleaning mould |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1351093A CN1351093A (en) | 2002-05-29 |
| CN1161415C true CN1161415C (en) | 2004-08-11 |
Family
ID=4593894
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB001299964A Expired - Fee Related CN1161415C (en) | 2000-10-30 | 2000-10-30 | Amino resin compositions for cleaning mould |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1161415C (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104194645B (en) * | 2014-08-07 | 2016-05-11 | 湖北迪曼特科技有限公司 | For removing clear mould cake and the preparation and application thereof of the residual aluminium of mould to be repaired |
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2000
- 2000-10-30 CN CNB001299964A patent/CN1161415C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN1351093A (en) | 2002-05-29 |
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