CN112680298A - Tableware detergent and laundry detergent taking soapstock as raw material and preparation method thereof - Google Patents
Tableware detergent and laundry detergent taking soapstock as raw material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a tableware detergent and laundry detergent taking soapstock as a raw material and a preparation method thereof, belonging to the technical field of daily chemicals. The invention prepares the higher fatty acid sodium by saponifying the soapstock, which comprises the following steps: (1) measuring the saponification value of the soapstock, and calculating the alkali addition amount of the saponification of the soapstock; (2) after the soapstock is melted, adding alkali in batches under the stirring state, and reacting for 2.5-5h under the slightly boiling state; (3) adding warm saturated salt solution for salting out, stirring and heating for a while, and observing the separation condition of water and soap; (4) stopping heating after salting out, standing, and discharging wastewater to obtain higher fatty acid sodium. The higher fatty acid salt is used as a formula component to prepare tableware detergent and laundry detergent, has excellent washing effect and has great application prospect. The preparation method is simple, and has the advantages of low price and environmental friendliness.
Description
Technical Field
The invention relates to the technical field of daily chemicals, in particular to a tableware detergent and a laundry detergent taking soapstock as a raw material and a preparation method thereof.
Background
Grease is one of the most important nutrients for human life and is the second most essential product second to food in daily life. China is a country with large oil and fat demand, the oil and fat industry is an important component of the grain and oil food industry in China, and has very important status and function in national economy, in 2007, the annual output of vegetable oil in China is nearly 2000 ten thousand tons, the annual output of fish oil is about 3 ten thousand tons, and the annual output of fish oil is increased year by year.
With the increasing production of refined oil, the production of oil and fat refining byproducts is also increasing. The soapstock is a byproduct with recycling value, is separated from the free fatty acid in the crude oil removed by alkaline solution in the alkali refining deacidification process to neutralize the free fatty acid into fatty acid salt, and the total amount of the soap stock accounts for 5-6% of the oil yield. During the process of separating soapstock, part of impurities such as neutral oil, fatty acid and pigment are entrained, and the components of the impurities are approximately: the soap comprises 8-27% of neutral oil (glyceride), 30-40% of soap (sodium fatty acid), the balance of water, and a small amount of free fatty acid, phospholipid, lipoid, pigment and other substances, wherein the total fatty acid content is up to 40-60%, but the effective ingredients in the soapstock are not fully developed and utilized at present, the effective recycling rate is low, although the soap product which takes the soapstock as the raw material exists at present, the soap product belongs to the category of low-grade soap in industrial application, the content of effective active substances is low, the cleaning effect is extremely poor, the daily cleaning requirement cannot be met, and the types of other cleaning products which take the soapstock as the raw material are not reported.
Based on the above situation, how to realize the efficient recycling of soapstock and meet the requirements of different washing environments is a technical problem to be solved urgently at present.
Disclosure of Invention
The invention aims to provide a tableware detergent and a laundry detergent which take soapstock as raw materials and a preparation method thereof, which are used for solving the problems in the prior art, efficiently utilizing the soapstock which is a byproduct of grease alkali refining, and simultaneously ensuring that the prepared tableware detergent and the laundry detergent have excellent washing effect.
In order to achieve the purpose, the invention provides the following scheme:
one of the purposes of the invention is to provide a method for preparing higher fatty acid sodium by saponification of soapstock, which comprises the following steps:
(1) measuring the saponification value of the soapstock, and calculating the alkali addition amount of the saponification of the soapstock;
the saponification value of the soapstock is calculated according to the formula (I):
in formula (I):
c-actual concentration of hydrochloric acid standard solution (mol/L);
V2blank test consumes volume (mL) of hydrochloric acid solution;
V1-the volume of hydrochloric acid solution consumed by the test sample (mL);
m-soapstock mass (g);
56.11-molar mass of potassium hydroxide;
the alkali addition amount calculation formula of the soapstock re-saponification is shown as the formula (II):
in formula (II):
m is the mass (kg) of solid base required for 1t of oil;
s-average saponification value of the mixed oil;
n-purity (%) of solid caustic soda;
(2) after the soapstock is melted, adding alkali in batches under the stirring state, and reacting for 2.5-5h under the slightly boiling state;
(3) adding saturated salt solution of 30-40 deg.C for salting out, stirring, and heating for reaction for 2-3 min;
(4) stopping heating after salting out, standing, and discharging lower layer wastewater to obtain higher fatty acid sodium.
In the step (2) of the present invention, the calculated excess of the actual alkali addition amount relative to the alkali addition amount is 8%.
Further, the base is sodium hydroxide.
Further, the standing time in the step (4) is 2.5-6 h.
The invention also provides a dish washing detergent which comprises the following raw materials in percentage by mass:
wherein the higher fatty acid sodium is prepared by the preparation method.
The invention also aims to provide a preparation method of the dish detergent, which comprises the following steps:
adding 1/2 addition amount of deionized water into the higher fatty acid sodium, adding fatty alcohol-polyoxyethylene ether sulfate, dodecyl sulfate, alkylolamide and sodium alkyl benzene sulfonate in batches under stirring condition, adding sodium chloride and sodium benzoate after completely dissolving, supplementing the residual amount of deionized water to the required volume, and stirring for reaction for 0.5-1 h;
wherein the temperature of 1/2 deionized water added into the sodium higher fatty acid is 58-62 ℃; the sodium salt of higher fatty acid, fatty alcohol-polyoxyethylene ether sulfate, dodecyl sulfate, alkylolamide and sodium alkyl benzene sulfonate are used as surfactants, sodium chloride is used as a thickening agent, and sodium benzoate is used as a preservative.
The invention aims to provide a laundry detergent which comprises the following raw materials in percentage by mass:
the higher fatty acid sodium is prepared by the preparation method.
The fifth purpose of the invention is to provide a preparation method of the laundry detergent, which comprises the following steps:
adding 1/2 addition amount of deionized water into the higher fatty acid sodium, adding the fatty alcohol-polyvinyl ether and the sodium alkyl benzene sulfonate in batches under the stirring condition, adding triethanolamine and anhydrous sodium citrate after all the materials are dissolved, supplementing the residual amount of deionized water to the required volume, and stirring for reaction for 0.5-1 h;
wherein the temperature of 1/2 deionized water added into the sodium higher fatty acid is 58-62 ℃; the sodium higher fatty acid, the fatty alcohol-polyvinyl ether and the sodium alkyl benzene sulfonate are used as surfactants, the triethanolamine is used as a thickening agent, and the sodium benzoate is used as a preservative.
The invention discloses the following technical effects:
the method converts the residual neutral oil in the soapstock of the grease alkali refining byproduct into the high-grade fatty acid salt by re-saponification, fully utilizes the soapstock of the grease alkali refining byproduct, ensures the high-efficiency retention of active substances, has simple and controllable preparation process, is suitable for large-scale production, and has extremely high economic value. The dish washing detergent and the laundry detergent prepared by taking the higher fatty acid sodium after saponification of the soapstock as the raw material have high total active substances and excellent washing effect.
The invention takes the high-grade fatty acid salt obtained by saponifying the nigre again as the formula component to prepare the tableware detergent and the laundry detergent, replaces the expensive chemical raw materials in the traditional formula, and the high-grade fatty acid salt extracted from the nigre belongs to the anionic surfactant and has synergistic action with other surfactants, thereby ensuring the excellent washing effect of the formula product and having great application prospect.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but as a more detailed description of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. Further, for numerical ranges in this disclosure, it is understood that each intervening value, between the upper and lower limit of that range, is also specifically disclosed. Every smaller range between any stated value or intervening value in a stated range and any other stated or intervening value in a stated range is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference herein for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the present disclosure without departing from the scope or spirit of the disclosure. Other embodiments will be apparent to those skilled in the art from consideration of the specification. The specification and examples are exemplary only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are open-ended terms that mean including, but not limited to.
The "parts" in the present invention are all parts by mass unless otherwise specified.
The saponification value of the soapstock sample of the present invention was determined as follows:
1. the determination step comprises:
2g of soapstock sample (accurate to 0.0001g) is weighed in an erlenmeyer flask, 25.0mL of potassium hydroxide ethanol solution is added, a reflux condenser tube is connected, and the mixture is placed in a boiling water bath for heating and refluxing for 1 h. Stopping heating, slightly cooling, adding 5-10 drops of phenolphthalein indicator, and titrating with a hydrochloric acid standard solution when the indicator is hot until pink disappears. Meanwhile, 25.0mL of potassium hydroxide ethanol solution is sucked to carry out a blank test according to the same method.
2. And (4) calculating a result:
in formula (I):
c-actual concentration of hydrochloric acid standard solution (mol/L);
V2blank test consumes volume (mL) of hydrochloric acid solution;
V1-the volume of hydrochloric acid solution consumed by the test sample (mL);
m-soapstock mass (g);
56.11-molar mass of potassium hydroxide;
the alkali addition amount calculation formula of the soapstock re-saponification is shown as the formula (II):
in formula (II):
m is the mass (kg) of solid base required for 1t of oil;
s-average saponification value of the mixed oil;
n-purity (%) of solid caustic soda.
The actual alkali addition amount of the invention is 8% in excess of the calculated alkali addition amount.
Example 1
A tableware detergent taking soapstock as a raw material comprises the following components in percentage by mass:
the preparation method comprises the following steps:
(1) taking the soapstock of the grease alkali refining byproduct, detecting the saponification value of the soapstock, and calculating the alkali addition amount of the saponification of the soapstock;
(2) putting the soapstock into a reactor, heating the soapstock under the condition of oil bath at 100 ℃ to melt the soapstock, then adding alkali in batches under the stirring state, and reacting for 2.5 hours under the micro-boiling state;
(3) adding warm saturated salt solution at 30 deg.C for salting out, stirring and heating for 3min, and observing water and soap separation condition;
(4) salting out is repeatedly carried out twice, heating is stopped after even stirring, the materials are poured into a separating funnel and are kept stand for 6 hours, and then lower-layer wastewater is discharged, so that a soap base (higher fatty acid sodium) is obtained;
(5) adding deionized water (1/2 in amount) at 62 deg.C into a reactor, adding surfactant, thickener and antiseptic under stirring at 200rmp, adding deionized water to required volume, and maintaining stirring state for 0.5 hr to obtain dish washing detergent containing soapstock as raw material.
And (4) detecting that the medium-high grade fatty acid sodium of the soap base obtained in the step (4) is mainly sodium oleate, sodium linoleate, sodium palmitate, sodium stearate and sodium linolenate.
The total active content and detergency of the dishwashing detergent prepared in this example were determined according to the national standard GB/T9985-.
The detection result is as follows: the total active matter content is 16.4 percent and is higher than the national standard by 15 percent; the national standard dish washing detergent is used for washing 1.8 dishes in 250mg/L hard water, and the dish washing detergent is used for washing 3.8 dishes and 3.5 dishes in 250mg/L hard water and 400mg/L hard water respectively.
Example 2
A tableware detergent taking soapstock as a raw material comprises the following components in percentage by mass:
the preparation method comprises the following steps:
(1) taking the soapstock of the grease alkali refining byproduct, detecting the saponification value of the soapstock, and calculating the alkali addition amount of the saponification of the soapstock;
(2) putting the soapstock into a reactor, heating the soapstock under the condition of oil bath at 100 ℃ to melt the soapstock, then adding alkali in batches under the stirring state, and reacting for 5 hours under the micro-boiling state;
(3) adding warm saturated salt solution at 40 deg.C for salting out, stirring for 2min, and observing water and soap separation condition;
(4) salting out is repeatedly carried out twice, heating is stopped after even stirring, the materials are poured into a separating funnel and are kept stand for 3.5 hours, and lower-layer wastewater is discharged to obtain a soap base (higher fatty acid sodium);
(5) adding deionized water (1/2 in amount) at about 58 deg.C into a reactor, adding surfactant, thickener and antiseptic under stirring at 200rmp, adding deionized water to required volume, and maintaining stirring state for 1 hr to obtain dish washing detergent containing soapstock as raw material.
The total active content and detergency of the dishwashing detergent prepared in this example were determined according to the national standard GB/T9985-.
The detection result is as follows: the total active matter content is 17.2 percent and is higher than the national standard by 15 percent; the national standard dish washing detergent is used for washing 1.8 dishes in 250mg/L hard water, and the quantity of the dish washing detergent is 3.5 dishes and 4.0 dishes in 250mg/L hard water and 400mg/L hard water respectively.
Example 3
A tableware detergent taking soapstock as a raw material comprises the following components in percentage by mass:
the preparation method comprises the following steps:
(1) taking the soapstock of the grease alkali refining byproduct, detecting the saponification value of the soapstock, and calculating the alkali addition amount of the saponification of the soapstock;
(2) putting the soapstock into a reactor, heating the soapstock under the condition of oil bath at 100 ℃ to melt the soapstock, then adding alkali in batches under the stirring state, and reacting for 3 hours under the micro-boiling state;
(3) adding warm saturated salt solution of 35 deg.C for salting out, stirring and heating for 2.5min, and observing water and soap separation condition;
(4) salting out is repeatedly carried out twice, heating is stopped after even stirring, the materials are poured into a separating funnel and are kept stand for 4 hours, and lower-layer wastewater is discharged to obtain a soap base (higher fatty acid sodium);
(5) adding deionized water (1/2 in amount) at 60 deg.C into a reactor, adding surfactant, thickener and antiseptic under stirring at 200rmp, adding deionized water to required volume, and maintaining stirring state for 0.8 hr to obtain dish washing detergent containing soapstock as raw material.
The total active content and detergency of the dishwashing detergent prepared in this example were determined according to the national standard GB/T9985-.
The detection result is as follows: the total active matter content is 17 percent and is higher than the national standard by 15 percent; the national standard dish washing detergent is used for washing 1.8 dishes in 250mg/L hard water, and the dish washing detergent is used for washing 3.8 dishes and 3.5 dishes in 250mg/L hard water and 400mg/L hard water respectively.
Example 4
The liquid laundry detergent taking soapstock as a raw material comprises the following components in percentage by mass:
the preparation method comprises the following steps:
(1) taking the soapstock of the grease alkali refining byproduct, detecting the saponification value of the soapstock, and calculating the alkali addition amount of the saponification of the soapstock;
(2) putting the soapstock into a reactor, heating the soapstock under the condition of oil bath at 100 ℃ to melt the soapstock, then adding alkali in batches under the stirring state, and reacting for 3 hours under the micro-boiling state;
(3) adding warm saturated salt solution of 35 deg.C for salting out, stirring and heating for 3min, and observing water and soap separation condition;
(4) salting out is repeatedly carried out twice, heating is stopped after even stirring, the materials are poured into a separating funnel and are kept stand for 4 hours, and lower-layer wastewater is discharged to obtain a soap base (higher fatty acid sodium);
(5) deionized water (1/2 of the adding amount) with the temperature of about 60 ℃ is filled in a reactor, surfactant, thickener and preservative are added in batches under the stirring of 200rmp, the deionized water is added to the required volume, and the stirring state is maintained for 0.5h, thus obtaining the laundry detergent taking soapstock as the raw material.
The detergency of the laundry liquids prepared in examples 4 to 6 of the present invention was measured according to the national standard GB/T13174-2008 "measurement of detergency and circulating detergency of detergents for clothing" and GB/T13174-2008 "measurement of detergency and circulating detergency of detergents for clothing" modification No. 1:
cutting the artificial dirty cloth JB-03 (sebum dirty cloth) into circular test pieces with diameter of 6cm, measuring a laundry detergent sample by using 3 pieces, and respectively marking and measuring the whiteness value before washing. And (3) putting the dirty cloth with the measured whiteness into the prepared washing liquid, washing, rinsing, dehydrating, airing, and measuring the whiteness value after washing. And calculating the decontamination value (Ri) and the decontamination ratio (Pi) of the sample and the standard laundry detergent according to the recorded whiteness values before and after washing, and comparing.
(when Pi is more than or equal to 1.0, the result is that the detergency of the sample on the ith dirty cloth is equal to or superior to that of standard washing powder, the detergency of the ith dirty cloth is qualified for short; when Pi is less than 1.0, the result is that the detergency of the sample on the ith dirty cloth is inferior to that of standard washing liquid, the detergency of the ith dirty cloth is unqualified for short; and when Pi is more than 0.90 and less than 1.10, the repeated measurement (the total number of measurement is even) is needed to ensure the correctness of the measurement result.)
The soil release value ratio (Pi) of the laundry detergent of this example was measured to be 1.016.
Example 5
The liquid laundry detergent taking soapstock as a raw material comprises the following components in percentage by mass:
the preparation method comprises the following steps:
(1) taking the soapstock of the grease alkali refining byproduct, detecting the saponification value of the soapstock, and calculating the alkali addition amount of the saponification of the soapstock;
(2) putting the soapstock into a reactor, heating the soapstock under the condition of oil bath at 100 ℃ to melt the soapstock, then adding alkali in batches under the stirring state, and reacting for 5 hours under the micro-boiling state;
(3) adding warm saturated salt solution at 38 deg.C for salting out, stirring and heating for 2min, and observing water and soap separation condition;
(4) salting out is repeatedly carried out twice, heating is stopped after even stirring, the materials are poured into a separating funnel and are kept stand for 3.5 hours, and lower-layer wastewater is discharged to obtain a soap base (higher fatty acid sodium);
(5) and (3) filling deionized water (1/2 of the adding amount) with the temperature of about 58 ℃ into a reactor, adding a surfactant, a thickening agent and a preservative in batches under the stirring of 200rmp, supplementing the deionized water to the required volume, and maintaining the stirring state for 0.5h to obtain the laundry detergent taking the soapstock as the raw material.
The laundry detergent of this example was measured to have a decontamination value ratio (Pi) of 1.049 according to the test method of example 4.
Example 6
The liquid laundry detergent taking soapstock as a raw material comprises the following components in percentage by mass:
the preparation method comprises the following steps:
(1) taking the soapstock of the grease alkali refining byproduct, detecting the saponification value of the soapstock, and calculating the alkali addition amount of the saponification of the soapstock;
(2) putting the soapstock into a reactor, heating the soapstock under the condition of oil bath at 100 ℃ to melt the soapstock, then adding alkali in batches under the stirring state, and reacting for 2.5 hours under the micro-boiling state;
(3) adding warm saturated salt solution at 30 deg.C for salting out, stirring and heating for 3min, and observing water and soap separation condition;
(4) salting out is repeatedly carried out twice, heating is stopped after even stirring, the materials are poured into a separating funnel and are kept stand for 6 hours, and lower-layer wastewater is discharged to obtain a soap base (higher fatty acid sodium);
(5) deionized water (1/2 of the adding amount) with the temperature of about 62 ℃ is filled in a reactor, surfactant, thickener and preservative are added in batches under the stirring of 200rmp, the deionized water is added to the required volume, and the stirring state is maintained for 1h, thus obtaining the laundry detergent taking soapstock as the raw material.
The laundry detergent of this example was measured to have a soil release value ratio (Pi) of 1.022 according to the test method of example 4.
Comparative example 1
The difference from example 1 is that the higher sodium fatty acid obtained by saponification of the soapstock was replaced with a single sodium stearate.
The total active matter content of the dish washing detergent prepared by the comparative example is 11.2%, and the dish washing detergent is 1.5 and 2.1 in hard water of 250mg/L and 400mg/L respectively compared with the number of large washing plates.
Comparative example 2
The difference from example 4 is that the higher fatty acid sodium salt obtained by saponification of the soapstock was replaced with a single sodium oleate.
The test method prepared in this comparative example measured the laundry detergent of this example to have a stain removal value ratio (Pi) of 0.91.
Comparative example 3
The difference from example 1 is that the time of the slight boiling state in step (2) was adjusted to 5.3 hours.
The total active matter content of the dish washing detergent prepared by the comparative example is 11.4%, and the dish washing detergent is 1.6 and 2.2 respectively in hard water of 250mg/L and 400mg/L in terms of the number of large washing plates.
Comparative example 4
The difference from example 4 is that the time of the slight boiling state in the step (2) was adjusted to 5.3 hours.
The test method prepared in this comparative example measured the laundry detergent of this example to have a stain removal value ratio (Pi) of 0.93.
The above-described embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solutions of the present invention can be made by those skilled in the art without departing from the spirit of the present invention, and the technical solutions of the present invention are within the scope of the present invention defined by the claims.
Claims (7)
1. A method for preparing higher fatty acid sodium by saponification of soapstock is characterized by comprising the following steps:
(1) measuring the saponification value of the soapstock, and calculating the alkali addition amount of the saponification of the soapstock;
the saponification value of the soapstock is calculated according to the formula (I):
in formula (I):
c-actual concentration of hydrochloric acid standard solution (mol/L);
V2blank test consumes volume (mL) of hydrochloric acid solution;
V1-the volume of hydrochloric acid solution consumed by the test sample (mL);
m-soapstock mass (g);
56.11-molar mass of potassium hydroxide;
the alkali addition amount calculation formula of the soapstock re-saponification is shown as the formula (II):
in formula (II):
m is the mass (kg) of solid base required for 1t of oil;
s-average saponification value of the mixed oil;
n-purity (%) of solid caustic soda;
(2) after the soapstock is melted, adding alkali in batches under the stirring state, and reacting for 2.5-5h under the slightly boiling state;
(3) adding saturated salt solution of 30-40 deg.C for salting out, stirring, and heating for reaction for 2-3 min;
(4) stopping heating after salting out, standing, and discharging lower layer wastewater to obtain higher fatty acid sodium.
2. The method of preparing sodium higher fatty acid by saponification of soapstock according to claim 1, wherein the alkali is sodium hydroxide.
3. The method for preparing sodium higher fatty acid by saponification of soapstock according to claim 1, wherein the standing time in step (4) is 2.5-6 h.
4. The dish washing detergent is characterized by comprising the following raw materials in percentage by mass:
wherein the sodium higher fatty acid is prepared by the preparation method of any one of claims 1 to 3.
5. A process for preparing a dishwashing detergent according to claim 4, comprising the steps of:
adding 1/2 addition amount of deionized water into the higher fatty acid sodium, adding fatty alcohol-polyoxyethylene ether sulfate, dodecyl sulfate, alkylolamide and sodium alkyl benzene sulfonate in batches under stirring condition, adding sodium chloride and sodium benzoate after completely dissolving, supplementing the residual amount of deionized water to the required volume, and stirring for reaction for 0.5-1 h;
wherein the temperature of 1/2 deionized water added into the sodium higher fatty acid is 58-62 ℃.
6. The laundry detergent is characterized by comprising the following raw materials in percentage by mass:
the sodium higher fatty acid is prepared by the preparation method of any one of claims 1 to 3.
7. A method for preparing the laundry detergent of claim 6, comprising the steps of:
adding 1/2 addition amount of deionized water into the higher fatty acid sodium, adding the fatty alcohol-polyvinyl ether and the sodium alkyl benzene sulfonate in batches under the stirring condition, adding triethanolamine and anhydrous sodium citrate after all the materials are dissolved, supplementing the residual amount of deionized water to the required volume, and stirring for reaction for 0.5-1 h;
wherein the temperature of 1/2 deionized water added into the sodium higher fatty acid is 58-62 ℃.
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