CN109297778B

CN109297778B - High-flux sample preparation device for combined polyether

Info

Publication number: CN109297778B
Application number: CN201811169311.5A
Authority: CN
Inventors: 李明友; 魏光曦; 李欣; 念以亭
Original assignee: Shandong Inov New Material Co Ltd
Current assignee: Shandong Inov New Material Co Ltd
Priority date: 2018-10-08
Filing date: 2018-10-08
Publication date: 2021-10-19
Anticipated expiration: 2038-10-08
Also published as: CN109297778A

Abstract

The invention discloses a high-flux sample preparation device, which comprises at least two liquid supply parts, at least two metering parts and at least two sample preparation parts, wherein the outlet end of each liquid supply part is provided with an equivalent metering module, and each equivalent metering module is communicated with the sample preparation parts through the metering parts; the metering part comprises a difference metering module and a plurality of liquid inlet pipes which are arranged at the liquid inlet end of the difference metering module in parallel, and each liquid inlet pipe is provided with a liquid inlet branch pipe which is communicated with each equivalent metering module one by one; the difference metering module is internally provided with volume metering units which are communicated with the liquid inlet pipes in a one-to-one correspondence mode, and the outlet end of each volume metering unit is communicated with one sample preparation part. The high-throughput sample preparation device is used for research and development of the combined polyether polyol, and the formula screening efficiency of the combined polyether polyol can be improved and the material consumption and waste output of test work can be reduced by adopting the high-throughput sample preparation device.

Description

High-flux sample preparation device for combined polyether

Technical Field

The invention relates to the technical field of preparation research of compositions, in particular to a high-flux sample preparation device for preparing composite polyether.

Background

The combined polyether polyol is one of polyurethane raw materials and is commonly called white materials in the industry. It is mixed with polyisocyanate (commonly called 'black material') and formed into polyurethane high-molecular material with specific performance. Because the polyisocyanate has high molecular activity, the modification and adjustment difficulty of the polyisocyanate is high, and the final structural performance of the polyurethane product is highly dependent on the formula adjustment of the combined polyether polyol. The conventional combined polyether polyol experimental system has large material consumption, and the produced polyurethane foam material is difficult to directly treat, so that the preparation quantity of single samples is reduced on the basis of keeping the system stable, and the improvement of the preparation efficiency of the samples is very important for the formula research and development of the combined polyether polyol.

Disclosure of Invention

The invention aims to overcome the defects in the prior art, and provides a high-throughput sample preparation device for combined polyether, which is used for research and development work of combined polyether polyol.

In order to achieve the above purpose, the invention provides the following technical scheme:

a high-flux sample preparation device comprises at least two liquid supply parts, at least two metering parts and at least two sample preparation parts, wherein an outlet end of each liquid supply part is provided with an equivalent metering module, and each equivalent metering module is communicated with the sample preparation parts through the metering parts;

the metering part comprises a difference metering module and a plurality of liquid inlet pipes which are arranged at the liquid inlet end of the difference metering module in parallel, and each liquid inlet pipe is provided with a liquid inlet branch pipe which is communicated with each equivalent metering module one by one;

volume metering units which are correspondingly communicated with the liquid inlet pipes one by one are arranged in the difference metering module, and the outlet end of each volume metering unit is communicated with one sample preparation part;

after the liquid in at least one liquid supply part is distributed into a plurality of equal-amount solutions through the equal-amount metering module, the equal-amount solutions enter the difference metering module through the liquid inlet pipes in a one-to-one correspondence mode, the volume metering unit performs difference metering on each equal-amount solution, the equal-amount solutions are mixed with solutions which are distributed in other liquid supply parts in an equal-amount manner in a one-to-one correspondence mode, and the solutions enter the corresponding sample preparation parts to perform sample preparation.

Preferably: equivalent metering module is liquid equivalent distribution valve, liquid equivalent distribution valve includes the valve body, the entry end of valve body is equipped with the valve top of single passageway, and the exit end is equipped with the base of multichannel, the base is followed a plurality of tunnels have been seted up to the equidistant axial of valve body, the quantity in tunnel and every feed liquor branch pipe equivalent on the feed liquor pipe, just the tunnel with the sealed intercommunication of feed liquor pipe, and every all be equipped with resistance element in the tunnel.

Preferably: the resistance element is a capillary tube, and the diameter of the capillary tube is 50-800 μm.

Further: the diameter of the capillary tube is 80-300 μm.

Preferably: the valve body and the base are made of high polymer materials or metal materials, and the liquid inlet pipe is made of inert soft materials.

Further: the material of feed liquor pipe is inert to polyisocyanate, preferred silica gel.

Preferably: the volume metering unit is an accommodating device with equal diameter and unequal height or an accommodating device with equal height and unequal diameter.

Preferably: the material of the difference metering module is inert to polyisocyanate, and preferably polyethylene, polytetrafluoroethylene or silica gel.

Preferably: the outlet end of each volume metering unit is provided with a two-way valve, the lower part of each two-way valve is provided with two parallel branches, one parallel branch is communicated with the sample preparation part, and the other parallel branch is communicated with the liquid recovery device.

Preferably: the liquid supply part is connected with the equivalent metering module through a quick connector.

Preferably: the liquid supply part comprises a liquid storage part and a power unit, and the power unit is a manual injection device or a micro flow pump device.

Compared with the prior art, the invention has the following beneficial effects:

the invention provides a high-throughput sample preparation device which comprises a liquid supply part, a metering part and a sample preparation part, and realizes small-amount, efficient and accurate differential sample preparation by combining three modules. When the device is used, according to a chemical sample preparation principle, a fixed liquid and a modulation solution are firstly set, wherein the fixed liquid can be a single solution or a mixed solution (usually fixed is a mixture of multiple components) with a fixed proportion and needs to be prepared in advance; the solution to be conditioned is usually a single solution, but sometimes a mixture of components to be conditioned, also needs to be prepared beforehand. Because the invention has a plurality of liquid supply parts, so the optimization condition of chemical sample preparation is satisfied, two liquid supply parts are usually arranged, firstly, the modulation solution is pumped to the equivalent metering module corresponding to the modulation solution through the liquid supply parts and then enters the volume metering unit in the difference metering module through each liquid inlet branch pipe, and repeatable unequal volume metering can be obtained in different pipelines when the volume metering unit is filled with liquid; and then the fixed solution is equally distributed by the equivalent metering modules corresponding to the fixed solution and then enters each liquid inlet branch pipe, and then the fixed solution and the modulation solution in each volume metering unit cooperate to enter a sample preparation part for sample preparation, so that the function of adjustable components in sample preparation is realized.

Drawings

In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.

FIG. 1 is a schematic structural diagram of an embodiment of the present invention;

FIG. 2 is a schematic diagram of an equivalent metering module according to an embodiment of the present invention;

fig. 3 is a schematic structural diagram of a base of an equivalent metering module according to an embodiment of the present invention.

Description of reference numerals:

1. a liquid supply section; 2. a metering section; 21. a difference metering module; 211. a volume metering unit; 22. a liquid inlet pipe; 221. a liquid inlet branch pipe; 222. a three-way valve; 3. a sample preparation part; 4. an equivalent metering module; 41. a valve body; 42. a valve top; 43. a base; 431. a duct; 44. a resistance element; 5. a liquid recovery device; 6. a two-way valve; 7. and (4) parallel branches.

Detailed Description

The technical solutions of the present invention will be described clearly and completely with reference to the accompanying drawings, and it should be understood that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc., indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention. In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.

In addition, the technical features involved in the different embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.

As shown in fig. 1, the present invention provides a high throughput sample preparation device, which comprises at least two liquid supply parts 1, a metering part 2 and a sample preparation part 3, wherein an outlet end of each liquid supply part 1 is provided with an equivalent metering module 4, and each equivalent metering module 4 is communicated with the sample preparation part 3 through the metering part 2; the metering part 2 comprises a difference metering module 21 and a plurality of liquid inlet pipes 22 which are arranged at the liquid inlet end of the difference metering module 21 in parallel, and each liquid inlet pipe 22 is provided with a liquid inlet branch pipe 221 which is communicated with each equivalent metering module 4 one by one; the difference metering module 21 is internally provided with volume metering units 211 which are correspondingly communicated with the liquid inlet pipes 22 one by one, and the outlet end of each volume metering unit 211 is communicated with one sample preparation part 3; wherein, after the liquid in at least one liquid supply part 1 is distributed into a plurality of equal-amount solutions through the equal-amount metering module 4, the solutions correspondingly enter the difference metering module 21 through the liquid inlet pipes 22 one by one, the volume metering unit 211 performs difference metering on each equal-amount solution, and the solutions which are equivalently distributed in other liquid supply parts correspondingly one by one are mixed, and the mixed solution enters the corresponding sample preparation part 3 for sample preparation.

The invention provides a high-throughput sample preparation device, which comprises a liquid supply part 1, a metering part 2 and a sample preparation part 3, and realizes small-amount, efficient and accurate differential sample preparation by combining three modules. The combination of the equivalent metering module 4, the liquid inlet pipe 22 and the difference metering module 21 enables the invention to simultaneously realize the preparation of a plurality of samples with specific metering differences, when in use, according to the principle of chemical sample preparation, a fixed liquid and a modulation solution are firstly arranged, wherein the fixed liquid can be a single solution or a mixed solution (usually fixed is a mixture of a plurality of components) with fixed proportion, and needs to be prepared in advance; the solution to be conditioned is usually a single solution, but sometimes a mixture of components to be conditioned, also needs to be prepared beforehand. Because the invention has a plurality of liquid supply parts 1, so meet the optimization condition of chemical sample preparation, usually set up two liquid supply parts 1, pump the modulating solution to its correspondent equivalent metering module 4 through the liquid supply part first and then enter the volume metering unit 211 in the difference metering module 21 through each liquid inlet branch pipe 221, can obtain repeatable unequal volume metering in different pipelines when the volume metering unit 211 is full of liquid; then, the fixed solution is equally distributed by the equivalent metering module 4 corresponding to the fixed solution, and then enters each liquid inlet branch pipe 221, and then enters the sample preparation part 3 in cooperation with the modulation solution in each volume metering unit 211 to prepare a sample, so that the function of adjustable components in the sample preparation is realized.

The liquid supply part 1 comprises a liquid storage part and a power unit (not marked in the figure), the power unit can be a manual injection device or an electric injection device, such as a micro flow pump device, and in the invention, the liquid supply part 1 is connected with the equivalent metering module 4 by adopting a quick joint;

as shown in fig. 2, the equivalent metering module 4 is a liquid equivalent distribution valve, the liquid equivalent distribution valve includes a valve body 41, a valve top 42 with a single channel is disposed at an inlet end of the valve body 41, a base 43 with multiple channels is disposed at an outlet end of the valve body 41, as shown in fig. 3, the base 43 is provided with a plurality of holes 431 at equal intervals along an axial direction of the valve body 41, the number of the holes 431 is equal to that of the liquid inlet branch pipes 221 on each liquid inlet pipe 22, the holes 431 are in sealed communication with the liquid inlet pipes 22, and a resistance element is disposed in each hole 431. In this embodiment, the valve body 41 and the base 43 may be made of polymer material or metal material, such as polymer material, gypsum material, stainless steel, etc. which is easy to machine; the liquid inlet pipe 22 is made of inert soft material, such as silica gel or other material inert to polyisocyanate, the valve body 41 is preferably a cylinder with a diameter of 5-25cm and a height of 5-15cm, and the resistance element 44 can be a capillary tube with a diameter of 50-800 μm, preferably 80-300 μm. The high-throughput sample distribution device obtained under the size can realize equal distribution of liquid in different channels by the equal-quantity metering module 4 under the condition of providing an external power system, and when the quantity of the liquid distributed in any one parallel channel reaches 20g, the quantity difference of the liquid in other channels does not exceed 20 +/-0.1 g; the difference metering module 21 may dispense a determined volumetric amount of liquid into the different lines over 120 seconds, with the relative difference in the actual dispensed amounts of liquid in the different lines for multiple dispensing events being no greater than 0.1%.

Of course, in the present invention, the volume metering unit 211 may be a cylindrical container with equal or unequal heights, or a container with other shapes, as long as it has the function of differentially distributing the volumes of the solutions; the material of the difference metering module 211 may be any soft material that is inert to polyisocyanate, such as polyethylene, polytetrafluoroethylene, and silica gel.

In this embodiment, two liquid supply parts 1 are selected, one for conveying fixed liquid and one for conveying modulated liquid, and a three-way valve 222 is further disposed on the liquid inlet pipes 22 connected in parallel to the liquid inlet end of the difference metering module 21, and the three-way valve 222 is disposed at the connection of the liquid inlet branch pipes 221 of each liquid inlet pipe 22 to control the distribution sequence of the fixed liquid or the modulated liquid in equal amount, thereby avoiding disorder.

As a preferred embodiment, a two-way valve 6 may be disposed at the outlet end of each volume metering unit 211, and two parallel branches 7 may be disposed at the lower portion of the two-way valve 6, one parallel branch 7 being communicated with the sample preparation portion 3, and the other parallel branch 7 being communicated with the liquid recovery device 5. The configuration can improve the preparation efficiency of the invention, because the excessive modulation liquid can be directly filled into each volume metering unit 211, whether the volume metering units are full or not is not required to pay attention to, the two-way valve 6 is directly communicated with the liquid recovery device 5, the excessive modulation liquid can enter the liquid recovery device 5 through the two-way valve 6 and can be used for next sample preparation, the two-way valve 6 is switched to the sample preparation part 3 after each volume metering unit 211 is full, then the same amount of fixing solution is introduced into each volume metering unit 211, and the fixing solution and the modulation solution with different sampling amounts can enter the sample preparation part 3 together for sample preparation.

Experimental demonstration of the use of the device of the invention for dispensing liquids is given below:

the difference metering module can realize the differential preparation of a small amount of samples under the condition of matching with the power transmission module:

TABLE 1

Channel	1	2	3	4	5	6
							A1	0.4589	0.878	0.9125	1.0129	1.1987	1.4141
A2	0.4602	0.6915	0.9078	0.9912	1.2021	1.4025
							A3	0.4595	0.6898	0.9093	0.9945	1.2078	1.4102
RA,％	0.14	0.27	0.26	0.87	0.38	0.42
							B1	0.5268	0.7981	1.0471	1.1405	1.4023	1.6188
B2	0.5303	0.8054	1.0412	1.1452	1.3859	1.6235
							B3	0.5315	0.8032	1.0505	1.1500	1.3832	1.6244
RB,％	0.46	0.47	0.45	0.41	0.74	0.19

The weight of the liquid taken from the metering module after 9 cycles is shown in Table 1. Wherein A, B, C the medium used in the test is water, 20% NaCl solution, and the suffixes 1 and 2 represent the number of tests. Weighing was carried out using an electronic balance with a weight accuracy of 0.0001 g. The result shows that the metering deviation among different channels is not more than 1.0 percent, and the precision required by the formula development of the combined polyether polyol is met.

The equal-quantity distribution module can realize equal-quantity distribution of a small amount of samples in different channels under the condition of matching with the power transmission module:

TABLE 2

Channel	1	2	3	4	5	6	R,％
								A1	20.2412	20.1382	20.2386	20.1960	20.1760	20.1023	0.27
A2	31.7613	31.5981	31.6875	31.7095	31.5524	31.6829	0.24
								B1	26.1833	26.2202	26.1989	26.0015	26.0956	26.0871	0.32
B2	39.9291	39.7044	39.7581	39.6600	39.6712	39.9005	0.29

Table 2 shows the results of the 9 liquid aliquot testing solutions, each measuring the dispensed weight of liquid between different channels for a given total dosage. Wherein A, B, C the medium used in the test is water, 20% NaCl solution, and the suffixes 1 and 2 represent the number of tests. Weighing was carried out using an electronic balance with a weight accuracy of 0.0001 g. The result shows that the metering deviation among different channels is not more than 0.5 percent, and the precision required by the formula development of the combined polyether polyol is met.

And thirdly, the invention is used for research and development work, so the actual use effect depends on the specific formula preparation purpose and the test method, and the catalyst addition quantity and the reaction speed of the composition in the free foaming state are selected as examples (represented by representative time in different stages and commonly used in the industry).

TABLE 3

Table 3 shows the results of the sample preparation and foaming tests using a set of 6-channel sample preparation devices, in which the amount of catalyst was related to the rise, stringing, debonding time and density. The results show that the rise, stringing and debonding time of the sample system is obviously reduced along with the increase of the addition amount of the catalyst a, and the influence of the continuous increase on the rise, stringing and debonding time is weakened when the part of the catalyst a reaches 0.8. The above results are in line with the basic characteristics of catalyst a, while a reasonable "quantity-to-effect" relationship has been established for the use of catalyst a in this system, proving that the device according to the invention is effective.

(IV) the amount of the single sample prepared in (III) is 50.0 + -1.0 g, and the sample loss is reduced by nearly 50% compared with the conventional sample preparation amount of 150-200 g. The effective rate of the sample in the group of tests is 80%, and is improved by 1 time compared with the effective rate of the sample of 30-40% in the conventional sample preparation. The preparation time is reduced from the past 10-20 minutes/sample to 1-2 minutes/sample, and the sample preparation efficiency is improved by 1 order of magnitude.

The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.

Claims

1. A high-flux sample preparation device is characterized by comprising at least two liquid supply parts, at least two metering parts and a sample preparation part, wherein an outlet end of each liquid supply part is provided with an equivalent metering module, and each equivalent metering module is communicated with the sample preparation part through the metering part;

after the liquid in at least one liquid supply part is distributed into a plurality of equal-quantity solutions through the equal-quantity metering module, the equal-quantity solutions correspondingly enter the difference metering module one by one through the liquid inlet pipes, the volume metering unit performs difference metering on each equal-quantity solution, the equal-quantity solutions are correspondingly mixed with the solutions which are distributed in the other liquid supply parts in equal quantity one by one, and the solutions enter the corresponding sample preparation parts for sample preparation;

the outlet end of each volume metering unit is provided with a two-way valve, the lower part of each two-way valve is provided with two parallel branches, one parallel branch is communicated with the sample preparation part, and the other parallel branch is communicated with the liquid recovery device.

2. The high-throughput sampling device according to claim 1, wherein the equivalent metering module is a liquid equivalent distribution valve, the liquid equivalent distribution valve comprises a valve body, an inlet end of the valve body is provided with a valve top of a single channel, an outlet end of the valve body is provided with a multi-channel base, the base is provided with a plurality of channels at equal intervals along an axial direction of the valve body, the number of the channels is equal to that of the liquid inlet branch pipes on each liquid inlet pipe, the channels are communicated with the liquid inlet pipes in a sealing manner, and each channel is internally provided with a resistance element.

3. The high throughput sampling device of claim 2, wherein the resistive element is a capillary having a diameter of 50-800 μ ι η.

4. The high throughput sampling device of claim 3, wherein the diameter of the capillary is 80-300 μm.

5. The high throughput sampling apparatus of claim 2, wherein the valve body and the base are made of a polymer material or a metal material, and the liquid inlet pipe is made of an inert soft material.

6. The high throughput sampling apparatus of claim 2, wherein the material of the liquid inlet tube is inert to polyisocyanate.

7. The high throughput sampling device of claim 1, wherein the volumetric metering unit is a container with equal height and unequal diameter or a container with equal height and unequal diameter.

8. The high throughput sample preparation device according to claim 1, wherein the liquid supply portion and the equivalent metering module are connected by a quick connector.

9. The high throughput sampling apparatus of claim 1, wherein the liquid supply portion comprises a liquid storage portion and a power unit, the power unit being a manual injection apparatus or a micro flow pump apparatus.