Method for preparing liquid laundry condensate beads through continuous flow

Abstract

The invention discloses a method for preparing liquid laundry condensate beads by continuous flow, which comprises the following steps: respectively and simultaneously pumping deionized water and monoethanolamine into a micro-channel reactor 1 through a feed pump to obtain a mixed solution M1, and continuously feeding the mixed solution M1 into a micro-channel reactor P1; 1, 2-propylene glycol and sulfonic acid are pumped into the microchannel reactor 2 through a feeding pump at the same time to obtain a mixed solution M2, and then the mixed solution M2 is continuously fed into the microchannel reactor P1; respectively and simultaneously pumping FMEE and XL-8 into the micro-channel reactor 3 through a feeding pump to obtain a mixed solution M3, and continuously feeding the mixed solution M3 into the micro-channel reactor P2; respectively and simultaneously pumping AEO-7 and AEO-9 into the micro-channel reactor 4 through a feeding pump to obtain a mixed solution M4, and continuously feeding the mixed solution M4 into the micro-channel reactor P2; simultaneously pumping the mixed solution P1 and the mixed solution P2 flowing out of the micro-channel reactors P1 and P2 into a micro-channel reactor 7 through a continuous feeding pump to obtain liquid laundry condensate beads; the method is achieved through the micro-channel reactor, safety is achieved, the reaction mixing time is short, the technology is stable and reliable, the whole reaction process is easy to operate, the reaction progress is controllable, and continuous production of the liquid laundry condensate beads is achieved.

Description

Technical Field

[0001] The invention relates to the fields of detergent preparation and microfluidic technology, and in particular to a method for preparing a laundry condensate bead composition by utilizing microfluidic technology. Background Art

[0002] Green, concentrated, and easy to use are the main development directions of household liquid detergents. Laundry beads are made by coating super-concentrated liquid detergent with a water-soluble polymer film. They have a crystal-clear and fashionable appearance, accurate measurement, and are easy to use without hurting your hands. When the beads are placed in the washing machine, the outer film quickly dissolves in the water and releases the detergent wrapped in it to achieve the purpose of cleaning clothes. Due to the super-concentrated formula, a whole bucket of clothes usually only requires one or two laundry beads, and its efficiency is often higher than that of traditional laundry powder and laundry liquid. Therefore, laundry beads have also become an important direction for the adjustment and upgrading of my country's laundry product structure.

[0003] The preparation of traditional liquid laundry beads generally adopts the high-speed shear method. Usually, the various components are placed together in a container, and the high-speed shear generated by the high-speed rotation of the homogenizer rotor is used to finally obtain a uniform mixed system. Because the high-speed shear method will have a large number of bubbles in the preparation process, a long static defoaming process is required after preparation. Compared with the traditional shear emulsification technology, microfluidic technology has significant advantages in controlling the mixing process. The liquid laundry beads prepared by it are clear and transparent, and can be mass-produced through parallel amplification of microfluidic devices.

[0004] The preparation method of liquid laundry beads disclosed in the prior art is relatively complicated, requiring a lot of stirring and shearing to mix, and the preparation process cannot be continuous. Based on this, we propose a method for preparing liquid laundry beads, hoping to solve the shortcomings of the prior art. Summary of the invention

[0005] In order to overcome the shortcomings of the prior art, the present invention provides a method for preparing liquid laundry beads, which is prepared by connecting multiple microchannel reactors in series and parallel. The method has the characteristics of safety, short preparation time, stable and reliable process, simple operation, and continuity. At the same time, the liquid laundry beads produced have good effect and do not need to be allowed to stand for defoaming, which is an improvement over traditional synthesis methods.

[0006] In order to achieve the above object, the technical solution adopted by the present invention is:

[0007] A method for preparing liquid laundry beads in a continuous flow, comprising the following steps in sequence:

[0008] (1) Preparation of materials: prepare deionized water, monoethanolamine, 1,2-propylene glycol, sulfonic acid, fatty acid methyl ester ethoxylate FMEE, fatty alcohol polyether XL-80, fatty alcohol polyoxyethylene ether, fatty alcohol polyoxyethylene ether (N=9) AEO-9;

[0009] (2) Microchannel preparation of liquid laundry beads:

[0010] S1: The deionized water and monoethanolamine in step 1) are pumped into the lime glass channel reactor 1 through feed pumps to obtain a mixed solution M 1 , and then continuously fed to the microchannel reactor P1;

[0011] S2: The 1,2-propylene glycol and sulfonic acid in step 1) are pumped into the microchannel reactor 2 through feed pumps to obtain a mixed solution M 2 , and then continuously fed to the microchannel reactor P1;

[0012] S3: The FMEE and XL-8 in step 1) are pumped into the microchannel reactor 3 through feed pumps to obtain a mixed solution M 3 , and then continuously fed to the microchannel reactor P2;

[0013] S4: AEO-7 and AEO-9 in step 1) are pumped into the microchannel reactor 4 through feed pumps to obtain a mixed solution M. 4 , and then continuously fed to the microchannel reactor P2;

[0014] S5: The mixed solution P flowing out of the microchannel reactors P1 and P2 1 and mixed solution P 2 By continuously feeding into the microchannel reactor 7, liquid laundry beads are obtained.

[0015] In the technical solution provided in the present application, the microchannel reactors P1 and P2 are preferably made of soda-lime glass; the microchannel reactor 7 is preferably made of pressure-resistant 316L stainless steel.

[0016] Furthermore, in the above-mentioned method for preparing liquid laundry beads by continuous flow, the flow rate of the feed pump in step (2) S1 is controlled at 1.00-8.00 mL / min, and the residence time is 9-15 min.

[0017] Furthermore, in the above-mentioned method for preparing liquid laundry beads by continuous flow, the feed pump flow rate in step (2) S2 is controlled at 5.00-20.00 mL / min, and the residence time is 5-20 min.

[0018] Furthermore, in the above-mentioned method for preparing liquid laundry beads by continuous flow, the feed pump flow rate in step (2) S3 is controlled at 4.00-9.00 mL / min, and the residence time is 5-12 min.

[0019] Furthermore, in the above-mentioned method for preparing liquid laundry beads by continuous flow, the feed pump flow rate in step (2) S4 is controlled at 2.00-5.00 mL / min, and the residence time is 13-21 min.

[0020] Furthermore, in the above-mentioned method for preparing liquid laundry beads in a continuous flow, the mixed solution M 1 and mixed solution M 2 The flow rate ratio is 3:8, wherein the mixed flow rate is 25.00-45.00 mL / min and the residence time is 2-5 min.

[0021] Furthermore, in the above-mentioned method for preparing liquid laundry beads in a continuous flow, the mixed solution M 3 and mixed solution M 4 The flow rate ratio is 11:6, wherein the mixed flow rate is 15.00-25.00 mL / min and the residence time is 4-8 min.

[0022] Furthermore, in the above-mentioned method for preparing liquid laundry beads in a continuous flow, the mixed solution P 1 and mixed solution P 2 The flow rate ratio is 3.3:1.7, wherein the mixed flow rate is 40.00-65.00 mL / min and the residence time is 1-3 min.

[0023] Furthermore, the temperature during step (2) of the above-mentioned method for preparing liquid laundry beads by continuous flow is 25°C.

[0024] Furthermore, in the above-mentioned method for preparing liquid laundry beads by continuous flow, the pressure during step (2) is 101 kPa.

[0025] Furthermore, in the above-mentioned method for preparing liquid laundry beads by continuous flow, the liquid holding capacity of a single microchannel reactor in step (2) is 100 ml, and the overall reactor comprises 7 reactors in total.

[0026] Compared with the prior art, the present invention provides a method for preparing liquid laundry beads, which has the following beneficial effects:

[0027] 1. The technical solutions provided by the present invention are respectively used to prepare liquid laundry beads through a microchannel reactor. The method is safe, has a short preparation time, a stable and reliable process, simple operation, and can be produced continuously. At the same time, the liquid laundry beads produced have good effects and do not need to be allowed to stand for defoaming, which is an improvement over traditional synthesis methods.

[0028] 2. This method can synthesize liquid laundry beads of different proportions by adjusting the flow rate of the feed pump, which greatly improves the efficiency of the production process, saves manpower and material resources, and reduces production costs. BRIEF DESCRIPTION OF THE DRAWINGS

[0029] Figure 1 It is a schematic diagram of the overall structure of the method for preparing liquid laundry beads provided in the present application;

[0030] Figure 2 is: the appearance of the liquid laundry beads prepared in Example 1;

[0031] Figure 3 This is an appearance picture of the liquid laundry beads prepared in Comparative Example 1. DETAILED DESCRIPTION

[0032] The following will be combined with the process of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0033] Example 1

[0034] The present embodiment provides a liquid laundry detergent bead, comprising the following components in percentage by mass: 12% deionized water, 24% 1,2-propylene glycol, 6% monoethanolamine, 24% sulfonic acid, 8% FMEE, 14% XL-80, 4% AEO-7, and 8% AEO-9.

[0035] The liquid laundry beads are prepared by the following steps: Figure 1 .

[0036] S11: Deionized water and monoethanolamine were simultaneously pumped into the calcium glass channel reactor 1 at flow rates of 6 mL / min and 3 mL / min, respectively, with a residence time of 11.12 min to obtain a mixed solution M 1 , and then continuously fed to the soda-lime glass microchannel reactor P1;

[0037] S21: 1,2-propylene glycol and sulfonic acid were simultaneously pumped into the lime glass channel reactor 2 at flow rates of 12 mL / min and 12 mL / min, respectively, with a residence time of 4.17 min to obtain a mixed solution M 2 , and then continuously fed to the soda-lime glass microchannel reactor P1;

[0038] S31: FMEE and XL-80 were simultaneously pumped into the microchannel reactor 3 at flow rates of 4 mL / min and 7 mL / min, respectively, with a residence time of 9.09 min to obtain a mixed solution M 3 , and then continuously fed to the soda-lime glass microchannel reactor P2;

[0039] S41: AEO-7 and AEO-9 were simultaneously pumped into the microchannel reactor 4 at flow rates of 2 mL / min and 4 mL / min, respectively, with a residence time of 16.67 min to obtain a mixed solution M 4 , and then continuously fed to the soda-lime glass microchannel reactor P2;

[0040] S51: The mixed solution P flowing out of the soda-lime glass microchannel reactors P1 and P2 is 1 and mixed solution P 2 The liquid laundry beads were simultaneously pumped into the pressure-resistant 316L stainless steel microchannel reactor 7 through a continuous feed pump. The residence time in this stage was 18.92 min, and liquid laundry beads were obtained.

[0041] Example 2

[0042] The present embodiment provides a liquid laundry detergent bead, comprising the following components in percentage by mass: 14% deionized water, 24% 1,2-propylene glycol, 4% monoethanolamine, 24% sulfonic acid, 10% FMEE, 12% XL-80, 6% AEO-7, and 6% AEO-9.

[0043] The liquid laundry beads are prepared by the following steps:

[0044] S11: Deionized water and monoethanolamine were simultaneously pumped into the microchannel reactor 1 at flow rates of 5.6 mL / min and 1.6 mL / min, respectively, with a residence time of 13.89 min to obtain a mixed solution M 1 , and then continuously fed to the soda-lime glass microchannel reactor P1;

[0045] S21: 1,2-propylene glycol and sulfonic acid were simultaneously pumped into the microchannel reactor 2 at flow rates of 9.6 mL / min and 9.6 mL / min, respectively, with a residence time of 5.21 min to obtain a mixed solution M 2 , and then continuously fed to the soda-lime glass microchannel reactor P1;

[0046] S31: FMEE and XL-80 were simultaneously pumped into the microchannel reactor 3 at flow rates of 4 mL / min and 4.8 mL / min, respectively, with a residence time of 11.37 min to obtain a mixed solution M 3 , and then continuously fed to the soda-lime glass microchannel reactor P2;

[0047] S41: AEO-7 and AEO-9 are simultaneously pumped into the microchannel reactor 4 at flow rates of 2.4 mL / min and 2.4 mL / min, respectively, with a residence time of 20.84 min, and then continuously fed into the soda-lime glass microchannel reactor P2;

[0048] S51: The mixed solution P flowing out of the soda-lime glass microchannel reactors P1 and P2 is 1 and mixed solution P 2 The liquid was simultaneously pumped into the pressure-resistant 316L stainless steel microchannel reactor 7 by a continuous feed pump. The residence time in this stage was 13.65 min, and liquid laundry beads were obtained.

[0049] Example 3

[0050] The present embodiment provides a liquid laundry detergent bead, comprising the following components in percentage by mass: 12% deionized water, 12% 1,2-propylene glycol, 6% monoethanolamine, 36% sulfonic acid, 8% FMEE, 14% XL-80, 4% AEO-7, and 8% AEO-9.

[0051] The liquid laundry beads are prepared by the following steps:

[0052] S11: Deionized water and monoethanolamine were pumped into the microchannel reactor 1 at flow rates of 7.5 mL / min and 3.75 mL / min respectively, with a residence time of 8.89 min to obtain a mixed solution M 1 , and then continuously fed to the soda-lime glass microchannel reactor P1;

[0053] S21: 1,2-propylene glycol and sulfonic acid were simultaneously pumped into the microchannel reactor 2 at flow rates of 15 mL / min and 15 mL / min, respectively, with a residence time of 3.34 min to obtain a mixed solution M 2 , and then continuously fed to the soda-lime glass microchannel reactor P1;

[0054] S31: FMEE and XL-80 were simultaneously pumped into the microchannel reactor 3 at flow rates of 5 mL / min and 8.75 mL / min, respectively, with a residence time of 7.28 min to obtain a mixed solution M 3 , and then continuously fed to the soda-lime glass microchannel reactor P2;

[0055] S41: AEO-7 and AEO-9 were simultaneously pumped into the microchannel reactor 4 at flow rates of 2.5 mL / min and 5 mL / min, respectively, with a residence time of 13.34 min to obtain a mixed solution M 4 , and then continuously fed to the soda-lime glass microchannel reactor P2;

[0056] S51: The mixed solution P flowing out of the soda-lime glass microchannel reactors P1 and P2 is 1 and mixed solution P 2 The liquid was simultaneously pumped into the pressure-resistant 316L stainless steel microchannel reactor 7 by a continuous feed pump. The residence time in this stage was 8.74 min, and liquid laundry beads were obtained.

[0057] Example 4

[0058] The present embodiment provides a liquid laundry detergent bead, comprising the following components in percentage by mass: 14% deionized water, 12% 1,2-propylene glycol, 4% monoethanolamine, 36% sulfonic acid, 10% FMEE, 12% XL-80, 6% AEO-7, and 6% AEO-9.

[0059] The liquid laundry beads are prepared by the following steps:

[0060] S11: Deionized water and monoethanolamine were pumped into the microchannel reactor 1 at the flow rates of 7 mL / min and 2 mL / min respectively, and the residence time was 11.12 min to obtain a mixed solution M 1 , and then continuously fed to the soda-lime glass microchannel reactor P1;

[0061] S21: 1,2-propylene glycol and sulfonic acid were simultaneously pumped into the microchannel reactor 2 at flow rates of 6 mL / min and 18 mL / min, respectively, with a residence time of 4.17 min to obtain a mixed solution M 2 , and then continuously fed to the soda-lime glass microchannel reactor P1;

[0062] S31: FMEE and XL-80 were simultaneously pumped into the microchannel reactor 3 at flow rates of 5 mL / min and 6 mL / min, respectively, with a residence time of 9.10 min to obtain a mixed solution M 3 , and then continuously fed to the soda-lime glass microchannel reactor P2;

[0063] S41: AEO-7 and AEO-9 were simultaneously pumped into the microchannel reactor 4 at flow rates of 3 mL / min and 3 mL / min, respectively, with a residence time of 16.67 min to obtain a mixed solution M 4 , and then continuously fed to the soda-lime glass microchannel reactor P2;

[0064] S51: The mixed solution P flowing out of the soda-lime glass microchannel reactors P1 and P2 is 1 and mixed solution P 2 The liquid laundry beads were simultaneously pumped into the pressure-resistant 316L stainless steel microchannel reactor 7 through a continuous feed pump. The residence time in this stage was 10.93 min, and liquid laundry beads were obtained.

[0065] Comparative Example 1

[0066] Based on Example 1, its formula components and dosage are the same as those of Example 1. The difference from Example 1 is that the preparation method is conventional stirring.

[0067] The liquid laundry beads are prepared by the following steps:

[0068] (1) According to the above mass fractions, deionized water and 1,2-propylene glycol were stirred for 10 minutes to dissolve;

[0069] (2) Add monoethanolamine and sulfonic acid, stir for 20 minutes, and after complete dissolution, raise the solution temperature to 55°C;

[0070] (3) Add FMEE, XL-80, AEO-7, and AEO-9 and stir for 40 min until completely dissolved;

[0071] (4) After stirring evenly, let it stand for 60 minutes, cool to room temperature and let it stand to defoam until it becomes clear and transparent.

[0072] In order to demonstrate the advantages of the technical solution provided by the present application, experimental data of the technical solution provided by the present application are given below.

[0073] Determination of stain removal performance:

[0074] According to the national standard GB / T13174-2021 method, a surfactant solution with a mass fraction of 0.2% was prepared using 250 mg / L standard hard water. The vertical decontamination machine was used to conduct decontamination experiments on national standard dirty cloths JB-01, JB-02 and JB-03 at (30±1)°C. The whiteness of all dirty cloths before and after washing was tested using a whiteness meter and the difference was calculated. The decontamination index was calculated by dividing the whiteness difference of the test sample by the result of the standard laundry detergent. If the index is greater than or equal to 1, it means that the decontamination power meets the national standard requirements.

[0075] Table 1 Decontamination performance test results

[0076] serial number JB01 JB02 JB03 Standard laundry detergent ＝1 ＝1 ＝1 Example 1 >1 >1 >1 Example 2 >1 >1 >1 Example 3 >1 >1 >1 Example 4 >1 >1 >1 Comparative Example 1 >1 >1 >1

[0077] Table 1: The decontamination ability of the liquid laundry beads prepared in Examples 1, 2, 3, 4 and Comparative Example 1, respectively, is obtained from Table 1. The liquid laundry beads prepared using the microchannel reactor have a test concentration of 1 / 4 of the standard laundry detergent, and the decontamination ability is better than the standard laundry detergent, which meets the latest industry standard requirements for laundry beads. Therefore, the synthesis method for preparing liquid laundry beads using a microchannel reactor provided in this application is feasible.

[0078] Table 2 Performance of liquid laundry beads prepared by different methods

[0079]

[0080] Table 2 is a performance comparison of the liquid laundry beads prepared by this method and the liquid laundry beads of the same components prepared by conventional technology. Figure 3 It can be seen that the liquid laundry beads prepared by the synthesis method for continuously preparing liquid laundry beads provided in the present application have significantly improved appearance compared with conventionally prepared liquid laundry beads while having the same performance.

[0081] Table 3 Time required for preparing liquid laundry beads by different preparation methods

[0082]

[0083] Table 3 is a comparison of the time required for preparing liquid laundry beads by this method and the time required for preparing liquid laundry beads of the same components by conventional technology. It can be seen from Table 3 that the liquid laundry beads prepared by the synthesis method for continuously preparing liquid laundry beads provided in the present application have significantly improved preparation time compared with conventionally prepared liquid laundry beads under the condition of the same performance, and the entire preparation process is continuously controllable.

[0084] The above contents are merely examples and explanations of the structure of the present invention. The technicians in this technical field may make various modifications or additions to the specific embodiments described or replace them in a similar manner. As long as they do not deviate from the structure of the invention or exceed the scope defined by the claims, they should all fall within the protection scope of the present invention.

Claims

1. A method for preparing liquid laundry beads in a continuous flow, characterized in that: The steps are as follows: (1) Preparation of materials: prepare deionized water, monoethanolamine, 1,2-propylene glycol, sulfonic acid, fatty acid methyl ester ethoxylate FMEE, fatty alcohol polyether XL-80, fatty alcohol polyoxyethylene ether, fatty alcohol polyoxyethylene ether (N=9) AEO-9; (2) Microchannel preparation of liquid laundry beads: S1: The deionized water and monoethanolamine in step 1) are respectively fed into the lime glass channel reactor 1 through a feed pump to obtain a mixed solution M 1 , and then continuously fed to the microchannel reactor P1; S2: The 1,2-propylene glycol and sulfonic acid in step 1) are pumped into the microchannel reactor 2 through feed pumps to obtain a mixed solution M 2 , and then continuously fed to the microchannel reactor P1; S3: The FMEE and XL-8 in step 1) are pumped into the microchannel reactor 3 through feed pumps to obtain a mixed solution M 3 , and then continuously fed to the microchannel reactor P2; S4: AEO-7 and AEO-9 in step 1) are pumped into the microchannel reactor 4 through feed pumps to obtain a mixed solution M. 4 , and then continuously fed to the microchannel reactor P2; S5: The mixed solution P flowing out of the microchannel reactors P1 and P2 1 and mixed solution P 2 By continuously feeding into the microchannel reactor 7, liquid laundry beads are obtained.

2. A method for preparing liquid laundry beads in a continuous flow according to claim 1, characterized in that: The flow rate of the feed pump described in step (2) S1 is controlled at 1.00-8.00 mL / min, and the residence time is 9-15 min.

3. A method for preparing liquid laundry beads in a continuous flow according to claim 1, characterized in that: The flow rate of the feed pump described in step (2) S2 is controlled at 5.00-20.00 mL / min, and the residence time is 5-20 min.

4. A method for preparing liquid laundry beads in a continuous flow according to claim 1, characterized in that: The feed pump flow rate in step (2) S3 is controlled at 4.00-9.00 mL / min, and the residence time is 5-12 min.

5. A method for preparing liquid laundry beads in a continuous flow according to claim 1, characterized in that: The flow rate of the feed pump described in step (2) S4 is controlled at 2.00-5.00 mL / min, and the residence time is 13-21 min.

6. A method for preparing liquid laundry beads in a continuous flow according to claim 1, characterized in that: Step (2) S5: mixed solution M 1 and mixed solution M 2 The flow rate ratio is 3:8, wherein the mixed flow rate is 25.00-45.00 mL / min and the residence time is 2-5 min.

7. A method for preparing liquid laundry beads in a continuous flow according to claim 1, characterized in that: Step (2) S5: mixed solution M 3 and mixed solution M 4 The flow rate ratios are 11:6, respectively, wherein the mixed flow rate is 15.00-25.00 mL / min and the residence time is 4-8 min.

8. A method for preparing liquid laundry beads in a continuous flow according to claim 1, characterized in that: Step (2) S5: mixed solution P 1 and mixed solution P 2 The flow rate ratios are 3.3:1.7, respectively, wherein the mixed flow rate is 40.00-65.00 mL / min and the residence time is 1-3 min.

9. A method for preparing liquid laundry beads in a continuous flow according to claim 1, characterized in that: The temperature during step (2) is 25° C. and the pressure during the process is 101 kPa.

10. A method for preparing liquid laundry beads in a continuous flow according to claim 1, characterized in that: The liquid holding capacity of a single microchannel reactor in step (2) is 100 ml, and there are 7 microchannel reactors in total.

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