CN1092666C - Alkali penetrating agent - Google Patents
Alkali penetrating agent Download PDFInfo
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- CN1092666C CN1092666C CN 97120821 CN97120821A CN1092666C CN 1092666 C CN1092666 C CN 1092666C CN 97120821 CN97120821 CN 97120821 CN 97120821 A CN97120821 A CN 97120821A CN 1092666 C CN1092666 C CN 1092666C
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Abstract
To obtain the subject penetrant, capable of promoting the rapid and uniform penetration of an alkaline liquid and providing polyester-based fibers, undergoing the weight reduction processing and having an excellent gloss and drapeability by including a specific phosphoric ester (salt) and a sulfate ester (salt), etc., therein. This alkaline penetrant comprises (A) a phosphoric ester (salt) represented by formula I R<1> is a 1-6C aliphatic alkyl; AO is oxyethylene or oxypropylene; (n1 ) is 0-6; (n2 ) and (n3 ) are each 1 or 2; [(n2 )+(n3 )] is 3} and (B) a phosphoric ester (salt) represented by formula II [R<2> is a 7-9C aliphatic alkyl; (m1 ) is (n1 ); (m2 ) is (n2 ); (m3 ) is (n3 )] or a sulfate ester (salt) represented by formula III and further preferably (C) a phosphoric ester represented by formula IV [R<3> is a 1-6C aliphatic alkyl; R<4> is a 7-9C aliphatic alkyl; (s1 ) and (s2 ) are each 0-6]. Furthermore, the weight compounding ratio of the components A/B is preferably (70/30) to (97/3).
Description
The present invention relates to carrying out the permeate agent that decrement adds the use in man-hour with alkali lye processing polyester fiber.
Usually the polyester fiber class is treated to and has the same soft hand feeling of thin,tough silk, the method with desirable drape is to adopt alkali lye, particularly sodium hydroxide solution to carry out decrement treatment.It is that surface with polyester fiber is hydrolyzed in alkali lye, removes degradation production by washing with water, carries out the method for decrement.
This method has the mylar rolling at present, in aqueous sodium hydroxide solution, flood, the extension white silk method that long-time heating is handled, the method for in liquid-flow dyeing machine, handling, in the aqueous solution of alkali, flood, rolling afterwards, seal the volume method of padding of placement, or methods such as method are rolled in the steaming of carrying out decatize after dipping.
Add in these decrements and to use quaternary ammonium salt promoting agent as promotor usually man-hour, perhaps then added the permeate agent that is used for mercerising processing as the alkali lye permeate agent.But at the former, because powerful hydrolysis promoter action, greatly reduce intensity, and owing to residual cationic active agent arranged, in aftertreatment, can occur damaging and the problem of flavescence.And in the latter, have the shortcoming of damaging decrement processing.
Therefore, in order to address the above problem, in public clear 55-22587 communique of spy and the clear 55-148277 of Te Kai, use special phosphate and sulfuric ester are disclosed as alkali penetrating agent, but these alkali penetrating agents do not have the enough stability to alkali yet, and perviousness, the particularly sodium hydroxide perviousness deficiency in 15-25 weight % scope the time, can bring sub-economic problem owing to increase add-on.In these methods,, after having adjusted alkali penetrating agent, in operation, when preserving, sampling sharply reduced perviousness, very inconvenience when reality is used for alkaline stability.
Inventors of the present invention can promote alkali lye infiltration equably rapidly in order to provide, the polyester fiber class that decrement is processed has good gloss, feel, drape, intensity etc., and to the alkali penetrating agent of the stability and the superior permeability of alkali, result through studying intensively has finished the present invention for this reason.
That is to say and the present invention relates to contain (A) with the phosphoric acid ester of following general formula (I) expression or its salt and the sulfuric ester of (B) representing or the alkali penetrating agent of its salt with the phosphoric acid ester of following general formula (II) expression or its salt or with following general formula (III).
(in the formula, R
1The expression carbonatoms is 1～6 straight or branched aliphatic alkyl, and AO represents hydroxyalkyl vinyl base or hydroxypropyl thiazolinyl, n
1The integer of expression 0～6, n
2The integer of expression 1 or 2, n
3The integer of expression 1 or 2, n
2+ n
3Equal 3.)
(in the formula, R
2The expression carbonatoms is 7～9 side chain aliphatic alkyl, and AO represents hydroxyalkyl vinyl base or hydroxypropyl thiazolinyl, m
1The integer of expression 0～6, m
2The integer of expression 1 or 2, m
3The integer of expression 1 or 2, m
2+ m
3Equal 3.)
The invention still further relates to the alkali penetrating agent of the phosphoric acid ester that contains following general formula (IV) expression.
(in the formula, R
3The expression carbonatoms is 1～6 straight or branched aliphatic alkyl, R
4The expression carbonatoms is 7～9 side chain aliphatic alkyl, and AO represents hydroxyalkyl vinyl base or hydroxypropyl thiazolinyl, s
1And s
2The integer of expression 0～6.)
In other words, the present invention relates to by above-mentioned (A) and the alkali penetrating agent composition that (B) forms and contain the alkali penetrating agent of the phosphoric acid ester of general formula (IV) expression.
The short chain phosphoric acid ester of (A) and the medium chain phosphoric acid ester (B) or the combination of medium chain sulfuric ester just.And (IV) be to have short chain and medium-chain phosphoric acid ester.
Ideal (B) is sulfuric ester or its salt of general formula (III) expression.
R among general formula (I), (IV)
1, R
3It is desirable to carbonatoms and be the aliphatic alkyl of 1～4 straight or branched, or carbonatoms is 1 or 2 aliphatic alkyl.
(A) contain two or more at least different R sometimes
1
At first, to phosphoric acid ester or its salt that (A) the above-mentioned general formula (I) that is comprised in the alkali penetrating agent of the present invention is represented, (B) phosphoric acid ester or its salt of above-mentioned general formula (II) expression, sulfuric ester or its salt of perhaps above-mentioned general formula (III) expression describe.
(A) component can prepare industrial being easy to by conventional known method, for example by Vanadium Pentoxide in FLAKES (P
2O
5), oxygen phosphorus trichloride (POCl
3) or phosphorylation agent and general formula R such as polyphosphoric acid
1O (AO) n
1H (R
1, AO, n
1Identical with above-mentioned general formula (I)) reaction of the oxy-compound of expression and preparing.
(A) R in the component
1Be that carbonatoms is the aliphatic alkyl of 1～6 straight or branched, it is desirable to carbonatoms and be 1～4 straight or branched aliphatic alkyl.AO represents hydroxyalkyl vinyl base or hydroxypropyl thiazolinyl, and its addition mole number is 0～6 mole, it is desirable to the addition mole number and be 0～3 mole hydroxyalkyl vinyl base.Ester is phosphoric acid one ester or phosphodiester, can be single phosphoric acid one ester and phosphodiester, also can be both mixtures.And under the situation that is salt, can adopt basic metal and ammonia, Monoethanolamine MEA BASF, diethanolamine or trolamine etc. to contain the alkali of nitrogen as neutralizing agent.
(B) component is phosphoric acid ester or its salt of general formula (II) expression, also usually can be by known method in industrial preparation, for example by Vanadium Pentoxide in FLAKES (P
2O
5), oxygen phosphorus trichloride (POCl
3) or phosphorylation agent and general formula R such as polyphosphoric acid
2O (AO) m
1H (R
2, AO, m
1Identical with above-mentioned general formula (II)) reaction of the oxy-compound of expression and preparing.
(B) R of the phosphoric acid ester of component or its salt
2Be that carbonatoms is the aliphatic alkyl of 7～9 side chain, it is desirable to different heptyl (3-methyl hexyl or 5-methyl hexyl), 2-ethylhexyl, 3,5,5-trimethylammonium hexyl.Its reason is owing to when adopting straight chain aliphatics alkane, can occur the problem of bubble in operation.Say so in more detail because foam overflows from steeping vat and collection box, say so bad from operability and security aspect.That is to say angle from industrial utilization, as the raw material oxy-compound that adopts when preparation phosphoric acid ester of (B) component or the salt, adopt iso-heptanol (mixture of 3-methyl-n-amyl carbinol and 5-methyl-n-amyl carbinol), 2-Ethylhexyl Alcohol, 3,5,5-trimethylammonium alcohol is an ideal.AO is hydroxyalkyl vinyl base or hydroxypropyl thiazolinyl, and its addition mole number is 0～6 mole, and the hydroxyalkyl vinyl base that the addition mole number is 0～3 mole is an ideal.Ester is phosphoric acid one ester or phosphodiester, can adopt single phosphoric acid one ester or phosphodiester, also the two can be mixed and use.And adopt under the situation of salt, can use nitrogenous alkali such as basic metal and ammonia, Monoethanolamine MEA BASF, diethanolamine or trolamine etc. as neutralizing agent.
(B) component can be sulfuric ester or its salt of general formula (III) expression, also is usually can be by known method in industrial preparation, for example by sulfuric acid (H
2SO
4), sulfuric chlorohydrin (HSO
3Cl), sulphur trioxide (SO
3) wait sulfur acidizing reagent and general formula R
2O (AO) m
1H (R
2, AO, m
1Identical with above-mentioned general formula (III)) prepared in reaction of the oxy-compound of expression.
(B) R in the sulfuric ester of component or its salt
2Be that carbonatoms is the aliphatic alkyl of 7～9 side chain, it is desirable to different heptyl (3-methyl hexyl or 5-methyl hexyl), 2-ethylhexyl, 3,5,5-trimethylammonium hexyl.That is to say from the angle of industrial use same as described above, as the raw material oxy-compound that adopts when preparation sulfuric ester of (B) component or the salt, adopt iso-heptanol (mixture of 3-methyl-n-amyl carbinol and 5-methyl-n-amyl carbinol), 2-Ethylhexyl Alcohol, 3,5, the 5-trimethyl hexanol is an ideal.AO is hydroxyalkyl vinyl base or hydroxypropyl thiazolinyl, and its addition mole number is 0～6 mole, and the hydroxyalkyl vinyl base that the addition mole number is 0～3 mole is an ideal.And under the situation that adopts salt, can adopt nitrogenous bases such as basic metal and ammonia, Monoethanolamine MEA BASF, diethanolamine or trolamine as neutralizing agent.
In the present invention, can be with above-mentioned (A) component and (B) component mixing use.(A) component and (B) the weight ratio of mixture of component be (A)/(B)=70/30～97/3, it is desirable to 80/20～90/10.
Phosphoric acid ester or its salt that the above-mentioned general formula (IV) that is comprised in the alkali penetrating agent of the present invention is represented describes below.
The phosphoric acid ester of general formula (IV) expression or its salt also can be by known method in industrial preparations, for example by Vanadium Pentoxide in FLAKES (P
2O
5), oxygen phosphorus trichloride (POCl
3) or phosphorylation agent and general formula R such as polyphosphoric acid
3O (AO) s
1H (R
3, AO, s
1Identical with above-mentioned general formula (IV)) oxy-compound and the general formula R of expression
4O (AO) s
2H (R
4, AO, s
2Identical with above-mentioned general formula (IV)) reaction of the oxy-compound of expression and preparing.Zhi Bei phosphoric acid ester is the mixture of phosphoric acid one ester and phosphodiester like this, perhaps obtains the simplification compound of phosphoric acid one ester or phosphodiester, but in the present invention, any phosphoric acid ester can, in feed stage, it is desirable to can be with general formula R
3O (AO) s
1Oxy-compound that H represents and R
4O (AO) s
2The oxy-compound that H represents is with R
3O (AO) s
1H/R
4O (AO) s
2H=70/30～97/3 (weight ratio), better is, and 80/20～90/10 ratio is used.That is to say R
3O (AO) s
1Base and R
4O (AO) s
2It is ideal that base finally exists in mixture with aforementioned proportion.
With the phosphoric acid ester of general formula (IV) expression or the R in its salt
3Be that carbonatoms is 1～6 straight or branched aliphatic alkyl, it is desirable to carbonatoms and be 1～4 straight or branched aliphatic alkyl.R
4Be that carbonatoms is 7～9 side chain aliphatic alkyl, it is desirable to different heptyl (the 3-methyl is base or 5-methyl hexyl), 2-ethylhexyl, 3,5,5-trimethylammonium hexyl.That is to say from the angle of industrial use same as described above,, it is desirable to adopt iso-heptanol (mixture of 3-methyl-n-amyl carbinol and 5-methyl-n-amyl carbinol), 2-Ethylhexyl Alcohol, 3,5, the 5-trimethyl hexanol as the raw material oxy-compound.AO is hydroxyalkyl vinyl base or hydroxypropyl thiazolinyl, and its addition mole number is 0～6 mole, and the hydroxyalkyl vinyl base that the addition mole number is 0～3 mole is an ideal.And under the situation that is salt, can use nitrogenous alkali such as basic metal and ammonia, Monoethanolamine MEA BASF, diethanolamine or trolamine etc. as neutralizing agent.
Use alkali penetrating agent of the present invention, the polyester fiber class is carried out decrement processing can be by past 3～40 weight %, it is desirable to add in the aqueous sodium hydroxide solution of 15～30 weight % the alkali penetrating agent of 0.1～1 weight %, flood the cloth of making by polyester fiber therein, squeeze into 30～100 weight %, pad in the operation 20～60 ℃ of placements 10～78 hours at volume, roll in the operation 100～160 ℃ of High Temperature High Pressure (HP) of carrying out 2～30 minutes in steaming and to handle, perhaps carry out heat (HT) decatize and wait and carry out.This also can adopt the extension of other impregnateds to practice method.
In the alkali lye of high density, add present addition and be 1/3～1/5 wetting agent, just can reach soft hand feeling.
Polyester fiber of the present invention is the material of being made by trevira, is meant the blended union material of blended union material, polyester and (three) acetic ester of finger polyethylene terephthalate and normal polyester fiber, cation-dyeable look trevira, cellulose fibre especially.
Specifically describe the present invention below, but the present invention is not limited to these embodiment.And " part " among the following embodiment and " % " represents " weight part " and " weight % " respectively.
At first, phosphoric acid ester or its salt of representing by the synthetic general formula (I) of following synthetic method.Synthesis example 1
15 parts of glycol-ethers and 15 parts of ethanol are joined in the reactor, slowly add 30 parts of Vanadium Pentoxide in FLAKESs at 45 ℃.After adding, temperature is risen to 60～70 ℃, under this temperature, stirred 4 hours.It is slowly joined in the reactor of another sodium hydroxide that has added 45 part 48% and 15 parts of water, neutralize being lower than under 40 ℃ the temperature, obtain compd A.Synthesis example 2
48 parts of ethylene glycol-butyl ethers and 72 parts of ethanol are joined in the reactor, slowly add 102 parts of Vanadium Pentoxide in FLAKESs at 40 ℃.After adding, temperature is risen to 60～70 ℃, under this temperature, stirred 4 hours.It is slowly joined in another reactor that has added 75 parts of sodium hydroxide (solid) and 151 parts of water, neutralize being lower than under 40 ℃ the temperature, obtain compd B.Synthesis example 3
120 parts of triethylene glycol-ether and 32 parts of methyl alcohol are joined in the reactor, slowly add 142 parts of Vanadium Pentoxide in FLAKESs at 45 ℃.After adding, stirred 3 hours at 45～50 ℃.It is slowly joined another 100 parts of sodium hydroxide (tablet) are dissolved in 197 parts of reactors in the water, neutralize being lower than under 40 ℃ the temperature, obtain Compound C.Synthesis example 4
90 parts of glycol-ethers are joined in the reactor, slowly add 47 parts of Vanadium Pentoxide in FLAKESs at 45 ℃.After adding, under 45～50 ℃ temperature, stirred 3 hours.It is slowly joined another 40 parts of sodium hydroxide (tablet) are dissolved in 88 parts of reactors in the water, neutralize being lower than under 40 ℃ the temperature, obtain Compound D.Synthesis example 5
90 part of one propylene glycol monoethyl ether joined in the reactor, slowly add 47 parts of Vanadium Pentoxide in FLAKESs at 45 ℃.After adding, under 45～50 ℃ temperature, stirred 3 hours.It is slowly joined another 40 parts of sodium hydroxide (tablet) are dissolved in 88 parts of reactors in the water, neutralize being lower than under 40 ℃ the temperature, obtain compd E.
Used sulfuric ester or its salt below are described.Synthesis example 6
130 parts of 2-ethylhexyl ethers are joined in the reactor, under the pressure of 15～20 ℃ temperature, 200～500mmHg, when stirring, add 115 parts of sulfuric chlorohydrins.After adding, under this temperature, removed hydrogen chloride gas 1 hour.
The 138 parts of water of packing in the neutralizing well, and add 40 parts of sodium hydroxide (tablet) dissolving, be cooled to below 20 ℃.Add above-mentioned sulfation material lentamente in this aqueous sodium hydroxide solution and neutralize, obtaining effectively part being 60% compound F 17-hydroxy-corticosterone.Synthesis example 7
109 parts of two-ethylene glycol, one 2-ethylhexyl ether is joined in the reactor, under the pressure of 15～20 ℃ temperature, 200～500mmHg, when stirring, add 58 parts of sulfuric chlorohydrins.After adding, under this temperature, removed hydrogen chloride gas 1 hour.
The 87 parts of water of packing in the neutralizing well, and add 28 parts of sodium hydroxide (tablet) dissolving, be cooled to below 20 ℃.Slowly add above-mentioned sulfation material in this aqueous sodium hydroxide solution and neutralize, obtaining effectively part being 60% compound G.Synthesis example 8
116 parts of iso-heptanols are joined in the reactor,, when stirring, add 115 parts of sulfuric chlorohydrins under 15～20 ℃ the temperature, under the pressure of 200～500mmHg.After adding, under this temperature, removed hydrogen chloride gas 1 hour.
The 230 parts of water of packing in the neutralizing well, and add 149 parts of trolamines dissolvings, be cooled to below 20 ℃.Slowly add above-mentioned sulfation material in this trolamine aqueous solution and neutralize, obtaining effectively part being 60% compound H.Synthesis example 9
130 parts of n-Octanols are joined in the reactor,, when stirring, add 115 parts of sulfuric chlorohydrins under 15～20 ℃ the temperature, under the pressure of 200～500mmHg.After adding, under this temperature, removed hydrogen chloride gas 1 hour.
The 138 parts of water of packing in the neutralizing well, and add 40 parts of sodium hydroxide (tablet) dissolving, be cooled to below 20 ℃.Add above-mentioned sulfation material lentamente in this aqueous sodium hydroxide solution and neutralize, obtaining effectively part being 60% Compound I.Synthesis example 10
85 parts of n-hexyl alcohols are joined in the reactor,, when stirring, add 115 parts of sulfuric chlorohydrins under 15～20 ℃ the temperature, under the pressure of 200～500mmHg.After adding, under this temperature, removed hydrogen chloride gas 1 hour.
The 84 parts of water of packing in the neutralizing well add 56 parts of sodium hydroxide (tablet) dissolving, are cooled to below 20 ℃.Add above-mentioned sulfation material lentamente in this aqueous sodium hydroxide solution and neutralize, obtaining effectively part being 60% compound J.Synthesis example 11
102 parts of n-hexyl alcohols and 97 parts of thionamic acids and 100 parts of dimethyl formamides are joined in the reactor, stirred 3 hours at 100 ℃.After reaction finishes, with methane amide underpressure distillation and recovery.Afterwards, add 25% ammoniacal liquor, with pH regulator to 7.The 132 parts of water of packing in the neutralizing well add above-mentioned sulfation material lentamente when stirring, obtaining effectively part being 60% compound K.Synthesis example 12
158 parts of nonylcarbinols are joined in the reactor,, when stirring, add 115 parts of sulfuric chlorohydrins under 15～20 ℃ the temperature, under the pressure of 200～500mmHg.After adding, under this temperature, removed hydrogen chloride gas 1 hour.
In neutralizing well, add 122 parts of water, and add 40 parts of sodium hydroxide (tablet) dissolving, be cooled to below 20 ℃.Add above-mentioned sulfation material lentamente in this aqueous sodium hydroxide solution and neutralize, obtaining effectively part being 60% compound L.
By the synthetic general formula (II) of the method shown in the synthesis example below or (IV) phosphoric acid ester or its salt of expression, or do not contain phosphoric acid ester or its salt of side chain.Synthesis example 13
44 parts of Diethylene Glycols, one 2-ethylhexyl ether is joined in the reactor, slowly add 14 parts of Vanadium Pentoxide in FLAKESs at 50 ℃.Under 45～50 ℃ temperature, stirred 3 hours after adding, wear out.It is joined another lentamente 8.8 parts of sodium hydroxide (tablet) are dissolved in 38 parts of reactors in the water, neutralize being lower than under 40 ℃ the temperature, obtain compound M.Synthesis example 14
24 parts of Diethylene Glycol-ether and 4.4 parts of Diethylene Glycol one 2-ethylhexyl ethers are joined in the reactor, add 13 parts of Vanadium Pentoxide in FLAKESs lentamente at 50 ℃.Under 45～50 ℃ temperature, stirred 3 hours after adding, wear out.It is joined another lentamente 8.8 parts of sodium hydroxide (tablet) are dissolved in 27 parts of reactors in the water, neutralize being lower than under 40 ℃ the temperature, obtain compound N.Synthesis example 15
39 parts of n-Octanols are joined in the reactor, add 14 parts of Vanadium Pentoxide in FLAKESs lentamente at 50 ℃.Under 45～50 ℃ temperature, stirred 3 hours after adding, wear out.It is joined another lentamente 8.0 parts of sodium hydroxide (tablet) are dissolved in 31.2 parts of reactors in the water, neutralize being lower than under 40 ℃ the temperature, obtain compound O.
List the embodiment that above-mentioned phosphoric acid ester or its salt and sulfuric ester or its salt is carried out performance evaluation below.
A/F, B/F, D/H, C/H are (I) and combination (III), and E/M is (I) and combination (II).Embodiment 1 (infiltrative evaluation)
Cut the trilateral of 1 centimetre of size from concise mylar (slim), in diameter is 7 centimetres culture dish, floating on the surface of sodium hydroxide permeate agent with each solution of concentration dissolved (30 milliliters) shown in the table 1 with concentration shown in the table 1, under 20 ℃ temperature, measure the complete wetted time (second) of cloth.This operation is carried out 40 times, and the mean value of last 5 times measured value is penetration time.The results are shown in table 1.
Table 1
| Impregnability test: unit (second) | NaOH15％ | NaOH20％ | NaOH25％ | NaOH30％ | |||||
| Permeate agent concentration | |||||||||
| 0.2％ | 0.5％ | 0.2％ | 0.5％ | 0.2％ | 0.5％ | 0.2％ | 0.5％ | ||
| Product of the present invention | Compd A/compound F 17-hydroxy-corticosterone (=90/10) (weight ratio) | 2 | 1 | 1 | 0.5 | 3 | 1 | 4 | 2 |
| Compd B/compound F 17-hydroxy-corticosterone (=95/5) (weight ratio) | 4 | 2 | 1 | 0.5 | 5 | 2 | 6 | 4 | |
| Compound D/compound H (=70/30) (weight ratio) | 2 | 1 | 2 | 1 | 2 | 1 | 2 | 1 | |
| Compound C/compound H (=80/20) (weight ratio) | 2 | 1 | 2 | 1 | 2 | 1 | 2 | 1 | |
| Compound C/compound G (=80/20) (weight ratio) | 6 | 3 | 5 | 3 | 5 | 3 | 8 | 5 | |
| Compd E/compound M (=90/10) (weight ratio) | 7 | 3 | 6 | 3 | 6 | 3 | 8 | 4 | |
| Comparative product | Compound N | 6 | 3 | 5 | 3 | 5 | 2 | 7 | 3 |
| Compd A | 214 | 79 | 47 | 15 | 6 | 2 | 5 | 0.8 | |
| Compd B | 231 | 67 | 41 | 13 | 16 | 6 | 12 | 4 | |
| Compound D | 203 | 59 | 21 | 8 | 3 | 1 | 3 | 0.6 | |
| Compound F 17-hydroxy-corticosterone | 0.4 | 0.4 | 0.5 | 0.5 | Can not measure | Can not measure | Can not measure | Can not measure | |
| Compound G | 3 | 2 | 10 | 5 | 18 | 9 | Can not measure | Can not measure | |
| Compound H | 0.4 | 0.4 | 0.4 | 0.4 | 10 | 3 | Can not measure | Can not measure | |
| Compound I | 0.7 | 0.4 | 0.5 | 0.4 | Can not measure | Can not measure | Can not measure | Can not measure | |
| Compd A/Compound I (=70/30) (weight ratio) | 5 | 2 | 4 | 2 | Can not measure | Can not measure | Can not measure | Can not measure | |
| Compd B/compound K (=50/50) (weight ratio) | More than 300 | 182 | More than 300 | 131 | 47 | 14 | 42 | 10 | |
| Compd A/Compound I (=80/20) (weight ratio) | 9 | 2 | 5 | 2 | Can not measure | Can not measure | Can not measure | Can not measure | |
| Compound D/compound L (=50/50) (weight ratio) | 15 | 8 | Can not measure | Can not measure | Can not measure | Can not measure | Can not measure | Can not measure | |
| Compound D/compound J (=75/25) (weight ratio) | 103 | 42 | 30 | 12 | 8 | 4 | 10 | 3 | |
Annotate) can not measure: since permeate agent can not be in aqueous sodium hydroxide solution uniform dissolution and can not measuring.Embodiment 2 (evaluation of alkaline stability)
To concentration is that to add concentration in 20% the aqueous sodium hydroxide solution be the permeate agent shown in 0.2% and 0.5% the table 2, places the perviousness of measuring each solution in 7 days afterwards down with 40 ℃ at once after modulation.Infiltrative measuring method is still identical with aforesaid method.The results are shown in table 2.
Table 2
Embodiment 3 (evaluation of whipability)
| Alkaline stability (seepage force experiment): unit (second) | Permeate agent concentration | ||||
| 0.2％ | 0.5％ | ||||
| At once afterwards | After 7 days | At once afterwards | After 7 days | ||
| Product of the present invention | Compd A/compound F 17-hydroxy-corticosterone (=90/10) (weight ratio) | 1 | 1 | 0.5 | 0.5 |
| Compound D/compound H (=70/30) (weight ratio) | 1 | 1 | 0.5 | 0.5 | |
| Compound C/compound G (=80/20) (weight ratio) | 1 | 1 | 0.5 | 0.5 | |
| Comparative product | Compd A | 47 | More than 300 | 15 | 49 |
| Compd B | 41 | More than 300 | 13 | 42 | |
| Compound D | 21 | 73 | 8 | 13 | |
| Compd A/compound L (=80/20) (weight ratio) | 30 | 82 | 10 | 30 | |
| Compd A/compound K (=95/5) (weight ratio) | 41 | 108 | 13 | 27 | |
In 1 liter graduated cylinder, adding 200 milliliters is the solution that has added 0.2% permeate agent in 20% the aqueous sodium hydroxide solution toward concentration, the employing internal diameter is 5 millimeters a Glass tubing, speed with 1.4 liters of per minutes is blown into air, is blown into back 15 seconds of beginning and measures foamy height (millimeter) after 180 seconds.The results are shown in table 3.
Table 3
| Whipability experiment: unit (millimeter) | After 15 seconds | After 180 seconds | |
| Product of the present invention | Compd A/compound F 17-hydroxy-corticosterone (=/ 10) (weight ratio) | 5 | 15 |
| Compound D/compound H (=70/30) (weight ratio) | 7 | 12 | |
| Comparative product | Compound D/compound O (=75/25) (weight ratio) | 25 | 60 |
| Compd A/Compound I (=90/10) (weight ratio) | 10 | 30 | |
| Compound C/compound L (=90/10) (weight ratio) | 15 | 45 | |
Claims (8)
1. alkali penetrating agent composition contains (A) with the phosphoric acid ester of following general formula (I) expression or its salt with (B) with phosphoric acid ester or its salt of following general formula (II) expression, and sulfuric ester or its salt of perhaps using following general formula (III) to represent form,
In the formula, R
1The expression carbonatoms is 1～6 straight or branched aliphatic alkyl, and AO represents oxygen ethylidene, n
1The integer of expression 0～3, n
2The integer of expression 1 or 2, n
3The integer of expression 1 or 2, n
2+ n
3Equal 3,
In the formula, R
2The expression carbonatoms is 7～9 side chain aliphatic alkyl, and AO represents oxygen ethylidene, m
1The integer of expression 0～3, m
2The integer of expression 1 or 2, m
3The integer of expression 1 or 2, m
2+ m
3Equal 3,, and wherein (A) component and (B) the weight ratio of mixture of component be (A)/(B)=70/30～97/3.
2. the alkali penetrating agent composition of claim 1 record, the R in its formula of (I)
1Be that carbonatoms is 1～4 the aliphatic alkyl of straight or branched.
3. the alkali penetrating agent that contains the phosphoric acid ester of following general formula (IV) expression,
In the formula, R
3The expression carbonatoms is 1～6 straight or branched aliphatic alkyl, R
4The expression carbonatoms is 7～9 side chain aliphatic alkyl, and AO represents oxygen ethylidene, s
1The integer of expression 0-3, s
2The integer of expression 0～6.
4. the alkali penetrating agent of claim 3 record, the R in its formula of (IV)
3Be that carbonatoms is 1～4 the aliphatic alkyl of straight or branched.
5. the alkali penetrating agents of claim 3 or 4 records, wherein in the phosphoric acid ester of general formula (IV) expression, R
3O (AO) s
1Base and R
4O (AO) s
2Base is with R
3O (AO) s
1Base/R
4O (AO) s
2The ratio of base=70/30～97/3 (weight ratio) exists.
6. the alkali penetrating agent composition of claim 1 record, wherein (B) is sulfuric ester or its salt of general formula (III) expression.
Claim 1 or 6 the record the alkali penetrating agent compositions, the R in its formula of (I)
1Be that carbonatoms is 1 or 2 aliphatic alkyl.
Claim 1 or 6 the record the alkali penetrating agent compositions, wherein (A) contains two or more at least different R
1
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP330582/96 | 1996-12-11 | ||
| JP8330582A JP2983917B2 (en) | 1996-12-11 | 1996-12-11 | Alkaline penetrant |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1193624A CN1193624A (en) | 1998-09-23 |
| CN1092666C true CN1092666C (en) | 2002-10-16 |
Family
ID=18234269
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 97120821 Expired - Lifetime CN1092666C (en) | 1996-12-11 | 1997-12-11 | Alkali penetrating agent |
Country Status (3)
| Country | Link |
|---|---|
| JP (1) | JP2983917B2 (en) |
| CN (1) | CN1092666C (en) |
| TW (1) | TW350002B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100839501B1 (en) * | 2002-04-30 | 2008-06-18 | 주식회사 코오롱 | A method of alkali treatment for woven or knitted fabric with composite fiber |
| CN109267397A (en) * | 2018-09-14 | 2019-01-25 | 桐乡市濮院毛针织技术服务中心 | A kind of purple dye bleeding agent of high density acrylic fabric |
-
1996
- 1996-12-11 JP JP8330582A patent/JP2983917B2/en not_active Expired - Lifetime
-
1997
- 1997-12-10 TW TW086118609A patent/TW350002B/en active
- 1997-12-11 CN CN 97120821 patent/CN1092666C/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JP2983917B2 (en) | 1999-11-29 |
| TW350002B (en) | 1999-01-11 |
| CN1193624A (en) | 1998-09-23 |
| JPH10168754A (en) | 1998-06-23 |
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| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
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| CX01 | Expiry of patent term |
Granted publication date: 20021016 |