CN102413889B

CN102413889B - Dewatering agent, dewatering method and dewatering device

Info

Publication number: CN102413889B
Application number: CN201080018815.2A
Authority: CN
Inventors: 松本省慈
Original assignee: Asahi Kasei Chemicals Corp
Current assignee: Tokuyama Metel Corp
Priority date: 2009-04-30
Filing date: 2010-04-30
Publication date: 2015-07-22
Anticipated expiration: 2030-04-30
Also published as: JP5627126B2; TW201100530A; MY156958A; TWI402337B; JPWO2010126130A1; WO2010126130A1; HK1165354A1; CN102413889A

Abstract

Disclosed are: a dewatering agent which exhibits good dewatering performance in removing water sticking to the surface of a subject to be washed, has a low toxicity and a low flammability and is free from the ozone depletion problem; a pre-rinsing agent; and a dewatering method and a dewatering device using the same. Specifically disclosed is a dewatering agent (a) containing a glycol ether [component (a1)] which lowers the solubility of water when liquid temperature is increased.

Description

Dehydrating agent, dewatering and dewater unit

Technical field

The present invention relates to and be suitable for removing the dehydrating agent of the moisture being attached to cleaned material surface, pre-washing agent, dewatering and dewater unit afterwards in the dehydration of precision instrument, optical instrument, electronic instrument and common metal parts etc.

Background technology

When dewatering after washing parts such as precision instrument, optical instrument, electronic instrument and common mechanical, extensive employing be carry out the method for pure water rinsing after with the suitable cleaning agent process corresponding to polluter, but finally to need the water removing existing for the article surface through cleaning.Carry out heating as dehydration means, reduce pressure, the physical method such as centrifugation, but from the viewpoint of dewatering is excellent, energy consumption cost is low, can rapid draing such, extensively universal is the dewatering of use solvent.

As solvent used during dehydration, isopropyl alcohol (hereinafter referred to as " IPA ") etc. can be enumerated.In addition also can by 3,3-bis-chloro-1,1,1,2,2-pentafluoropropane and 1,3-bis-chloro-1,1,2, the material adding ethanol, IPA or certain surfactant in the hydrochlorofluorocarazeotropics such as the mixture (hereinafter referred to as " HCFC225 ") of 2,3-pentafluoropropane or the chloro-1-fluoroethane of 1,1-bis-(hereinafter referred to as " HCFC141b ") uses (for example, see patent document 1 and patent document 2) as solvent.

But, due to problems such as depletions of the ozone layer, for HCFC225, HCFC141b, estimate to forbid that to the year two thousand twenty it uses.Therefore, motion is had to propose in non ozone depleting ability, the non-flame properties fluorine kind solvents such as the HFC class (hereinafter referred to as " HFC ") completely not containing chlorine atom or hydrogen fluorine ethers (hereinafter referred to as " HFE "), be added with ethanol or IPA dehydrating agent and dewatering (for example, see patent document 3) in recent years.

In addition, have motion to propose to utilize the dehydrating agent of glycol dialkyl ether and the method (for example, see patent document 4) to the water separation in dehydrating agent will be dissolved in by raising liquid temperature.

Further, the dehydrating agent of propylene glycol methyl ether acetate there is is motion to propose to utilize and by improving the method (for example, see patent document 5) that the water dissolved in is separated by liquid temperature.

Further, further, there is motion to propose and to the glycol ethers series solvent in fluorine kind solvent, add water to dissolving in, be separated into the method (for example, see patent document 6) of fluorine kind solvent and glycol ether solvent, water.

Prior art document

Patent document

Patent document 1: Japanese Unexamined Patent Publication 3-258734 publication

Patent document 2: Japanese Unexamined Patent Publication 4-334502 publication

Patent document 3: Japanese Unexamined Patent Publication 11-293285 publication

Patent document 4: Japanese Laid-Open Patent Publication 61-78401 publication

Patent document 5: Japanese Unexamined Patent Publication 9-255994 publication

Patent document 6: Japanese Unexamined Patent Publication 10-290963 publication

Summary of the invention

Invent problem to be solved

But, when using IPA as dehydrating agent, have that liquid exchange frequency is high, the low such problem of operating efficiency.In addition, because IPA is danger (flash-point: 12 DEG C), thus need dewater unit to make antiknock device, thus there is equipment cost increase such problem.

In the technology of patent document 3, owing to being added to shipwreck in dehydrating agent to be separated with ethanol or IPA when dewatering, thus there is dewatering and reduce such problem.So-called " being added to the water in dehydrating agent " be attached to cleaned material, fixture (ジグ), storage cleaned material the water etc. of basket etc. be dissolved into water in dehydrating agent when to dewater etc.

For the technology of patent document 4, because dehydrating agent is danger, thus need to make antiknock device on equipment.In addition, if utilize 1,1, chloro-1,2, the 2-HFC-143a of 2-tri-(hereinafter referred to as " CFC113 ") carries out rinsing to dehydrating agent, then dehydrating agent is accumulated in CFC113, has the problem occurring dry vestige on the surface of cleaned material owing to being added to the effect of the water in dehydrating agent simultaneously.

The technology of patent document 5 has following problem: except dehydrating agent is danger, owing to utilizing dimethyl carbonate (flash-point: 18 DEG C) to carry out vapour seasoning, because of but the high dewatering of fire hazard.In addition, owing to forming the state with water azeotropic, thus also have due to moisture contained in steam and produce the such problem of dry vestige on the surface of cleaned material.

In the technology of patent document 6, do not have to record about the content of the separation of dissolving in the water in dehydrating agent, having can not the such problem of the dewatering of long term maintenance dehydrating agent.

So, in the technology that the dehydration being representative with above-mentioned technology is relevant, exist and there is fire hazard, namely allow to dewater and also forbid that it uses or effectively the component separation be accumulated in dehydrating agent or purificant cannot be gone out such problem due to problems such as depletions of the ozone layer in the future.

The present invention proposes in view of the foregoing, its object is to dehydrating agent, pre-washing agent are provided, employ the dewatering of this dehydrating agent and dewater unit, described dehydrating agent is attached in the moisture on cleaned material surface in removing has excellent dewatering, for hypotoxicity, low inflammability, and without the need to worrying depletion of the ozone layer.

For solving the means of problem

The present inventor is studied dehydrating agent, pre-washing agent, the dewatering employing this dehydrating agent and dewater unit respectively in order to solve above-mentioned problem.Found that, for dehydrating agent, by making (a) dehydrating agent containing the glycol ethers (a1) making the dissolubility of water reduce by improving liquid temperature, not only there is excellent dewatering, and by adding the operations such as water if desired, flash-point can also be eliminated under the condition of dewatering keeping excellence.Find the liquid temperature by improving dehydrating agent, the water be added in dehydrating agent easily can be separated, and can eliminate flash-point.Further discovery, when using purificant, by reducing the liquid temperature of purificant, the dehydrating agent (a) be added in purificant easily can be separated, and isolated dehydrating agent parting liquid (c) can be used as pre-washing agent (ab), result obtains the rinsability of excellent dehydrating agent (a).Also find further, the composition of the isolated parting liquid containing dehydrating agent composition as dehydrating agent (a) can be recycled.

That is, the present invention is as follows.

[1] a kind of dehydrating agent (a), it contains the glycol ethers (composition (the a1)) solubility of water being reduced by improving liquid temperature.

[2] dehydrating agent (a) as described in [1], wherein, described composition (a1) is the compound shown in following formula (1).

R ¹O-(R ²O) _n-H (1)

(in formula, R ¹represent that carbon number is alkyl, the carbon number alkenyl that is 6 or 7, carbon number be 6 or 7 cycloalkyl, phenyl or benzyl, the R of 6 or 7 ²represent that carbon number is the alkylidene of 2 or 3, n represents the integer of 1 ~ 3.)

[3] dehydrating agent (a) as described in [1], wherein, described composition (a1) is diethylene glycol monohexyl ether or diethylene glycol list benzyl oxide.

[4] dehydrating agent (a) as described in [1], wherein, described composition (a1) is diethylene glycol list benzyl oxide.

[5] dehydrating agent (a) as described in any one of [1] ~ [4], wherein, this dehydrating agent (a) is further containing water (composition (a2)).

[6] dehydrating agent (a) as described in [5], wherein, the described composition (a1) of condition of this dehydrating agent (a) containing the meeting of 40 ~ 90 quality % following (i) and (ii) and described composition (a2) water of 60 ~ 10 quality %;

I when described composition (a1) carries out mixing with the ratio of mass ratio 1: 1 with described composition (a2) by (), if leave standstill at 10 ~ 30 DEG C, uniform dissolution, further, if leave standstill at 40 ~ 70 DEG C, upper strata (d) and lower floor (e) 2 layers are separated into;

(ii) (be 1.33 × 10 the vapour pressures of 20 DEG C by described composition (a1), described composition (a2) and composition (b1) ³the chlorine-free fluorine compounds of more than Pa) when carrying out mixing with the ratio of mass ratio 52: 3: 45, if leave standstill at 35 DEG C, uniform dissolution, and, if leave standstill at 15 DEG C, be separated into upper strata (f) and lower floor (g) 2 layers.

[7] dehydrating agent (a) as described in any one of [1] ~ [6], wherein, this dehydrating agent (a) is same composition with the lower floor (e) recorded in following condition (i);

I when described composition (a1) carries out mixing with the ratio of mass ratio 1: 1 with described composition (a2) by (), if leave standstill at 10 ~ 30 DEG C, uniform dissolution, further, if leave standstill at 40 ~ 70 DEG C, upper strata, upper strata (f) (d) and lower floor of lower floor (g) (e) 2 layers are separated into.

[8] a kind of pre-washing agent (ab), its contain the condition of meeting of 1 ~ 40 quality % following (iii), be 1.33 × 10 by what improve liquid temperature and the glycol ethers (composition (a1)) that makes the solubility of water reduce and 99 ~ 60 quality % the vapour pressure of 20 DEG C ³the chlorine-free fluorine compounds (composition (b1)) of more than Pa;

(iii) when described composition (a1) being carried out mixing with the ratio of mass ratio 1: 1 with water (a2), if leave standstill at 40 ~ 70 DEG C, be separated into upper strata (d) and lower floor (e) 2 layers, and, when by described lower floor (e) and described composition (b1) with 1: 1 mass ratio carry out mixing, in 25 DEG C standing, being separated into more than 2 layers that comprise its orlop (h).

[9] pre-washing agent (ab) as described in [8], wherein, this pre-washing agent (ab) is same composition with the described orlop (h) of described condition (iii).

[10] dewatering, it has following operation:

(1) dehydrating agent (a) described in any one of claim 1 ~ 7 is used, to the operation that cleaned material is dewatered;

(2) using containing composition (b1) (is 1.33 × 10 the vapour pressures of 20 DEG C ³the chlorine-free fluorine compounds of more than Pa) purificant (b), the cleaned material being attached with described dehydrating agent (a) is carried out to the operation of rinsing; And

(3) at least using the steam obtained by heating purificant (b), described cleaned material being carried out to the operation of vapour seasoning.

[11] dewatering as described in [10], wherein, the method has following operation further:

The described dehydrating agent (a) of water is had to heat to being dissolved in by described dehydration, thus by the operation removed at least partially of water contained in described dehydrating agent (a); And

The dehydrating agent (a) of water is eliminated, to the operation that described cleaned material is dewatered described in reusing.

[12] dewatering as described in [10] or [11], wherein, the method has following operation further:

Water is added to dissolving in have in the purificant (b) of dehydrating agent (a) by described rinsing, thus described dehydrating agent (a) contained in described purificant (b) is extracted in described water is separated, obtain the operation of dehydrating agent parting liquid (c);

Described dehydrating agent parting liquid (c) is heated, obtains the operation of the concentrate of described dehydrating agent parting liquid (c); And

Use described concentrate, described cleaned material is carried out to the operation of rinsing.

[13] dewatering as described in any one of [10] ~ [12], wherein, the method has following operation further:

The purificant (b) of dehydrating agent (a) is had to cool to being dissolved in by described rinsing, thus being separated at least partially described dehydrating agent (a) contained in described purificant (b), obtain the operation of dehydrating agent parting liquid (c);

[14] dewatering as described in any one of [10] ~ [12], wherein, the method has following operation further:

Water is added to dissolving in have in the purificant (b) of dehydrating agent (a) by described rinsing, thus described dehydrating agent (a) contained in described purificant (b) is extracted in described water, obtain the operation of the pre-washing agent (ab) containing dehydrating agent parting liquid (c);

Use described pre-washing agent (ab), described cleaned material is carried out to the operation of prewashing;

Described pre-washing agent (ab) is heated, obtains the operation of the concentrate of pre-washing agent (ab); And

At least use described concentrate, described cleaned material is carried out to the operation of rinsing.

[15] dewatering as described in [10], any one of [11] and [13], wherein, the method has following operation further:

After described (2) operation, the purificant (b) of dehydrating agent (a) is had to cool to dissolving in, a part for dehydrating agent (a) in purificant (b) is separated, obtains the operation of the pre-washing agent (ab) containing dehydrating agent parting liquid (c);

Use pre-washing agent (ab), the cleaned material being attached with dehydrating agent (a) is carried out to the operation of prewashing;

Pre-washing agent (ab) is heated, obtains the operation of the concentrate of pre-washing agent (ab); And

Use described concentrate, the cleaned material being attached with dehydrating agent (a) is carried out to the operation of rinsing.

[16] dewater unit, it possesses:

Use the drench pit that the dehydrating agent (a) described in any one of [1] ~ [7] dewaters to cleaned material;

Produce the distillation tank of purificant (b), pre-washing agent (ab) or the steam of both;

By in the concentrate of the described steam produced in described distillation tank except the water separating tank anhydrated;

Be used in the concentrate eliminating water in described water separating tank, described cleaned material carried out to the potcher of rinsing; And

Be used in described distillation tank the described steam produced, dry vapour seasoning portion is carried out to the described cleaned material through rinsing.

[17] dewater unit as described in [16], wherein, this device possesses further:

To the heating tank that described dehydrating agent (a) is heated; And

By the separating tank being separated water outlet in described dehydrating agent (a).

[18] dewater unit as described in [16] or [17], wherein, this device possesses further:

By adding water in described purificant (b), described dehydrating agent (a) being extracted in described water, obtaining the mixing channel of dehydrating agent parting liquid (c); And

The separating tank be separated with described purificant (b) to the described dehydrating agent (a) in described purificant (b) will be dissolved in.

[19] dewater unit as described in [16] or [17], wherein, this device possesses further:

By having the described purificant (b) of described dehydrating agent (a) to cool and being separated at least partially the described dehydrating agent (a) in described purificant (b) to dissolving in, obtain the cooling bath for dehydrating agent parting liquid (c) used in rinsing; And

To the separating tank that described purificant (b) is separated with dehydrating agent (a).

[20] dewater unit, it possesses:

At least be used in the described steam produced in distillation tank and dry vapour seasoning portion is carried out to cleaned material;

Described steam is made to cool the cooling end becoming concentrate;

By the water separating tank being separated water outlet in described concentrate;

Use the described concentrate being separated water, described cleaned material is carried out to the potcher of rinsing;

To dissolving in the heating tank having the described dehydrating agent (a) of water to heat;

By the first separating tank being separated water outlet in described dehydrating agent (a);

By to dissolve in have described dehydrating agent (a) described purificant (b) in add water and being extracted at least partially in water of the described dehydrating agent (a) in described purificant (b) removed, obtain the mixing channel of the pre-washing agent (ab) containing obtained dehydrating agent parting liquid (c);

To the second separating tank that described purificant (b) is separated with dehydrating agent (a);

Described pre-washing agent (ab) is utilized described cleaned material to be carried out to the prewash tank of prewashing; And

Described pre-washing agent (ab) is carried out to the liquor charging portion of liquor charging between described distillation tank and described prewash tank.

[21] dewater unit, it possesses:

At least be used in described distillation tank the described steam produced and dry vapour seasoning portion is carried out to cleaned material;

Described steam is made to cool the cooling end becoming concentrate;

By the first separating tank being separated water outlet in the described dehydrating agent (a) of heating in described heating tank;

There is the described purificant (b) of described dehydrating agent (a) to cool thus being separated at least partially the described dehydrating agent (a) in described purificant (b) to dissolving in, obtaining the cooling bath of the pre-washing agent (ab) containing obtained dehydrating agent parting liquid (c);

To the second separating tank that the purificant (b) carrying out described cooling is separated with dehydrating agent (a);

Invention effect

Utilize the present invention, dehydrating agent, pre-washing agent, the dewatering employing this dehydrating agent and dewater unit can be realized, described dehydrating agent is attached in the moisture on the surface of cleaned material in removing has excellent dewatering, is hypotoxicity, low inflammability, and without the need to worrying depletion of the ozone layer.

Accompanying drawing explanation

Fig. 1 is the schematic diagram of an example of the dewater unit of present embodiment.

Fig. 2 is the schematic diagram of another example of the dewater unit of present embodiment.

Fig. 3 is the schematic diagram of the another example of the dewater unit of present embodiment.

Fig. 4 is the schematic diagram of an example again of the dewater unit of present embodiment.

Fig. 5 is the schematic diagram of another example again of the dewater unit of present embodiment.

Fig. 6 is the schematic diagram of the example more again of the dewater unit of present embodiment.

Detailed description of the invention

Be described in detail to for implementing mode of the present invention (being hereafter only called " present embodiment ") with reference to accompanying drawing as required below.Following present embodiment is for illustration of example of the present invention, and not intended to be limits the invention to following content.Further, the present invention can want to carry out suitable distortion to implement in point range at it.In addition, in the accompanying drawings, same key element is composed with same symbol, omit repeat specification.In addition, for waiting position relationship up and down, only otherwise special declaration, then based on position relationship shown in the drawings.Further, the dimension scale of accompanying drawing is not limited to illustrated ratio.

In this manual, " dehydration " refer to and the water being attached to cleaned material be removed to the degree not affecting operation below." cleaned material " refers to the article cleaned by washing etc.

" rinsing " refers to and will extract in solvent at least partially containing what be attached to the dehydrating agent of water of cleaned material or pre-washing agent after dewatering." spray rinsing (shower rinse) " refers to the aqueous or vaporific solvent action that spues after dewatering in cleaned material, uses this solvent to carry out rinsing to the dehydrating agent being attached to cleaned material." prewashing " refers to after dewatering, before rinsing, by be attached to cleaned material, dehydrating agent containing water be extracted in solvent at least partially.

" vapour seasoning " refers in cleaned material, the dehydrating agent of minimal residue or pre-washing agent remove with the form of the liquid at cleaned material surface condensation on the surface by the temperature difference of cleaned material and steam.

" dehydrating agent parting liquid " refers to when carrying out standing separation to the liquid containing dehydrating agent becomes undermost liquid.

< dehydrating agent (a) >

The dehydrating agent (a) of present embodiment is containing the glycol ethers (a1) making the solubility of water reduce by improving liquid temperature.Glycol ethers (a1) is that 2 hydroxyl bonds are combined in aliphatic on 2 different carbon atoms or ester ring type compound, refer to 1 hydrogen in this hydroxyl by hydrocarbon residue or the hydrocarbon residue containing ehter bond the compound that replaces.

Glycol ethers (a1) is preferably the compound shown in following formula (1).

R ¹O-(R ²O) _n-H (1)

By containing the compound with structure shown in formula (1), utilize saturation moisture concentration to change this point along with liquid temperature, can eliminate flash-point under the condition keeping dewatering, the water that simultaneously can easily will be added in dehydrating agent is separated.And, utilize and be dissolved in the dehydrating agent concentration in purificant along with the liquid temperature of purificant and change this point, easily purificant can being separated with dehydrating agent, simultaneously by being used before rinsing process by isolated dehydrating agent parting liquid, excellent dehydrating agent can being obtained rinsability.

As the particular compound of glycol ethers (a1), such as ethylene glycol mono-n-butyl ether, ethylene glycol list isobutyl ether, diethylene glycol monohexyl ether, diethylene glycol list benzyl oxide, propane diols list positive propyl ether etc. can be enumerated.Among these, diethylene glycol monohexyl ether, diethylene glycol list benzyl oxide have excellent dewatering, are the compounds of excellence in the separation property of water and the separation property of purificant simultaneously.Further, because diethylene glycol list benzyl oxide meets the full terms of aftermentioned (i) ~ (iii), because of but the compound of the best for the pre-washing agent (ab) of the rinsability excellence of the dehydrating agent (a) that obtains dehydration property excellence and dehydrating agent, and be the compound that the separation property of the separation property of water and purificant is the most excellent.

Dehydrating agent (a) preferably further containing water (a2), and is more preferably non-flammable.By adding water (a2) in dehydrating agent (a), can fire hazard be reduced, eliminate flash-point further.The dehydrating agent of the danger do not belonged in fire service law can be made thus.Said " elimination flash-point " refers to herein, and utilize " the Cleveland open type " recorded in JIS K 2265 to measure, in each assay method, dehydrating agent is all confirmed as without flash-point (that is, non-flammable).

When making the dehydrating agent (a) containing water (a2), its manufacture method being not particularly limited, according to conventional method, water (a2) can being mixed with composition (a1), by carrying out homogenising to obtain.

When eliminating flash-point by making dehydrating agent (a) containing water (a2), as long as without detriment to high dehydration property, high-moisture from property, hypotoxic scope, be then not particularly limited mass ratio.Such as, when share glycol ethers (a1) with water (a2), the mass ratio of (a1)/(a2) is preferably the scope of 95/5 ~ 50/50.(a1) in the mass ratio of/(a2), by making the mass ratio of composition (a1) be less than 95/5, excellent elimination flash-point effect can be obtained.(a1), in the mass ratio of/(a2), by making the mass ratio of composition (a1) be more than 50/50, the residual of the water on cleaned material surface can be reduced.From the aspect of the balance of the residual of the water on the dehydration property of dehydrating agent and cleaned material surface, the scope of preferred mass ratio is 93/7 ~ 60/40.

The dehydrating agent (a) of present embodiment preferably contains the composition (a1) of condition meeting following (i) and (ii) and composition (a2) water of 60 ~ 10 quality % of 40 ~ 90 quality %.

(ii) (be 1.33 × 10 the vapour pressures of 20 DEG C by described composition (a1), described composition (a2) and composition (b1) ³the chlorine-free fluorine compounds of more than Pa) when carrying out mixing with the ratio of mass ratio 52: 3: 45, if leave standstill at 35 DEG C, uniform dissolution, and if leave standstill at 15 DEG C, be separated into upper strata (f) and lower floor (g) 2 layers.

By meeting above-mentioned condition (i) and (ii), in dehydration procedure described later, by liquid temperature being controlled to make water be dissolved in dehydrating agent with arbitrary ratio at 10 ~ 30 DEG C, thus excellent dewatering can be demonstrated.By liquid temperature is increased to 40 ~ 70 DEG C, can by dissolved water continuously and be easily separated with dehydrating agent, can the high dewatering of long term maintenance dehydrating agent.Further, because purificant demonstrates the rinsability of excellent rinsing dehydrating agent at 35 DEG C, thus by liquid temperature is reduced to 15 DEG C, purificant easily can be separated with dehydrating agent, can the excellent properties of long term maintenance purificant.

The so-called vapour pressure at 20 DEG C is 1.33 × 10 ³the part of the hydrogen atom that the chlorine-free fluorine compounds (b1) of more than Pa are hydro carbons or ethers only replace by fluorine atom, fluorine compounds not containing chlorine atom.Composition (b1) is not particularly limited, the ring-type HFC (HFC) such as shown in following formula (2), the chain HFC shown in following formula (3) and the hydrogen fluorine ether (HFE) shown in following formula (4) can be enumerated.Composition (b1) can be used alone a kind, also can be the combination of compound of more than two kinds.

C _nH _2n-mF _m(2)

(in formula, n and m represents the integer of relation of satisfied 4≤n≤6,5≤m≤2n-1.)

C _xH _2x+2-yF _y(3)

(in formula, x represents the integer of 4 ~ 6, and y represents the integer of 5 ~ 12.)

C _sF _2s+1OR (4)

(in formula, R represents that carbon number is the alkyl of 1 ~ 3, and s represents the integer of 4 ~ 6.)

As the concrete example of ring-type HFC, 3H can be enumerated, 4H, 4H-Freon C318,4H, 5H, 5H-Decafluorocyclopentane, 5H, 6H, 6H-nine fluorine cyclohexane etc.

As the concrete example of chain HFC, 1H can be enumerated, 1H, 1H, 3H, 3H-perfluorinated butane, 1H, 2H, 3H, 4H-perfluorinated butane, 1H, 2H-perfluorinated butane, 1H, 3H-perfluorinated butane, 2H, 3H-perfluorinated butane, 4H, 4H-perfluorinated butane, 1H, 1H, 3H-perfluorinated butane, 1H, 1H, 4H-perfluorinated butane, 1H, 2H, 3H-perfluorinated butane, 1H, 1H, 4H-perfluorinated butane, 1H, 2H-perflenapent, 1H, 4H-perflenapent, 2H, 3H-perflenapent, 2H, 4H-perflenapent, 2H, 5H-perflenapent, 1H, 2H, 3H-perflenapent, 1H, 3H, 5H-perflenapent, 1H, 5H, 5H-perflenapent, 2H, 2H, 4H-perflenapent, 1H, 2H, 4H, 5H-perflenapent, 1H, 4H, 5H, 5H, 5H-perflenapent, 1H, 2H-perflexane, 2H, 3H-perflexane, 2H, 4H-perflexane, 2H, 5H-perflexane, 3H, 4H-perflexane etc.

As the concrete example of HFE, methyl perfluoro butyl ether, methyl perfluoro isobutyl ether, methyl perfluoro amyl ether, methyl perfluoro hexamethylene ether, ethylperfluoro butyl ether, ethylperfluoro isobutyl ether, ethylperfluoro amyl ether etc. can be enumerated.

Preferably the middle lower floor (e) recorded is same composition to the dehydrating agent (a) of present embodiment with above-mentioned condition (i).By being this composition, when can be formed in described later use, recycle the more excellent material of property.

< purificant (b) >

When using the dehydrating agent (a) of present embodiment to dewater, purificant can be share.Be not particularly limited purificant operable in present embodiment, preferably using containing the vapour pressure at 20 DEG C is 1.33 × 10 ³the purificant (b) of the chlorine-free fluorine compounds (b1) of more than Pa.For purificant (b), by containing composition (b1), excellent drying property is demonstrated while replacement dewatering agent (a), thus cleaned material surface can be suppressed to produce dry vestige, require at optical lens etc. to use in the field of high dehydrating property.

For purificant (b), the one kind or two or more compound be selected from above-mentioned chlorine-free fluorine compounds (b1) can be combinationally used.Among these, such from the viewpoint of demonstrating good dissolution characteristics to glycol ethers monoalkyl ethers, preferred HFC or HFE, more preferably 1H, 1H, 1H, 3H, 3H-perfluorinated butane, 2H, 3H-perflenapent, methyl perfluoro butyl ether and methyl perfluoro isobutyl ether, ethylperfluoro butyl ether, ethylperfluoro isobutyl ether and their mixture.

The composition of purificant (b) is not particularly limited, consider from the aspect of the drying property improved further the final potcher before vapour seasoning, in purificant (b), the content of (a1) composition is preferably below 0.5 quality %, is more preferably below 0.1 quality %.Thereby, it is possible to improve the rinsability of the dehydrating agent containing water.

< pre-washing agent (ab) >

(a1) composition of the condition of pre-washing agent (ab) containing meeting of 1 ~ 40 quality % following (iii) of present embodiment and 99 ~ 60 quality %'s is 1.33 × 10 the vapour pressure of 20 DEG C ³the chlorine-free fluorine compounds (composition b1) of more than Pa.

(iii) by the lower floor (e) of above-mentioned condition (ii) and composition (b1) with 1: 1 mass ratio mix, in 25 DEG C standing when, be separated into more than 2 layers that comprise its orlop (h).

By meeting above-mentioned condition (iii), when using in dewatering described later and dewater unit, recirculation property is excellent, simultaneously can the prewashing performance of long term maintenance excellence.

In the present embodiment, also in the scope of the effect without detriment to present embodiment, the various auxiliary agents such as such as organic solvent, surfactant, stabilizing agent, defoamer, ultra-violet absorber can be added in dehydrating agent (a), purificant (b) and pre-washing agent (ab) as required.

As organic solvent, such as alcohols, ketone, ester class and hydro carbons etc. can be enumerated.As alcohols, methyl alcohol, ethanol, normal propyl alcohol, isopropyl alcohol etc. can be enumerated.As ketone, acetone, methyl ethyl ketone etc. can be enumerated.As ester class, Ethyl formate, carboxylic Acid Propyl, carboxvlic acid isobutyl, methyl acetate, ethyl acetate, methyl propionate, ethyl propionate etc. can be enumerated.As hydro carbons, n-hexane, isohexane, cyclohexane, cyclohexene, 2-methylpentane, 2,3-dimethylbutanes, normal heptane, 2-methyl hexane, 3-methyl hexane, 2,4-dimethyl pentanes, isooctane etc. can be enumerated.

As surfactant, such as anion system surfactant, cation system surfactant, nonionic surface active agent and amphoteric surfactant etc. can be enumerated.As anion system surfactant, alkali metal, alkanolamine and amine salt etc. that carbon number is the aliphatic acid, DBSA etc. of 6 ~ 20 can be enumerated.As cation system surfactant, quaternary ammonium salt etc. can be enumerated.As nonionic surface active agent, alkylphenol can be enumerated, the block polymer etc. of ethylene oxide adduct, polyoxyethylene and polyoxypropylene that carbon number is the aliphatic alcohol of the straight or branched of 8 ~ 18.As amphoteric surfactant, betaine type, amino acid pattern etc. can be enumerated.

As stabilizing agent, the such as nitroparaffin such as nitromethane, nitroethane hydro carbons can be enumerated; The epoxides such as 1,2-epoxy butane; The ethers such as Isosorbide-5-Nitrae-dioxane; The amines such as triethanolamine; 1,2,3-benzotriazole etc.By containing such stabilizing agent, can effectively prevent the burn into of cleaned material from getting rusty and variable color etc.

As defoamer, such as self-emulsifying silicone, silicon, aliphatic acid, higher alcohol, polypropylene glycol, polyethylene glycol and fluorine class surfactant etc. can be enumerated.

As ultra-violet absorber, such as benzophenone, phenyl salicylic acid esters class and benzotriazole etc. can be enumerated.

Next the dewatering and dewater unit that use above-mentioned dehydrating agent (a), purificant (b) and pre-washing agent (ab) etc. are described.In the present embodiment, as the dewatering and the dewater unit that use above-mentioned dehydrating agent (a) etc., being just not particularly limited as long as can dewater to cleaned material, can be any method and apparatus.Such as, directly can use the conventional dehydration methods and dewater unit etc. that utilize dehydrating agent (a), or also can carry out as required improveing to use.So, present embodiment does not limit the mode of dewatering and dewater unit, under regard to preferred dewatering and dewater unit in the dehydrating agent (a) etc. using present embodiment and be described.

< dewatering >

The dewatering of present embodiment has following operation:

Dehydration procedure (1): use above-mentioned dehydrating agent (a), the cleaned material that effects on surface is attached with water carries out the operation of dewatering;

Rinsing process (2): use is the purificant (b) of the chlorine-free fluorine compounds (b1) of 1.33 × more than 103Pa containing the vapour pressure at 20 DEG C, the cleaned material being attached with described dehydrating agent (a) is carried out to the operation of rinsing;

Vapour seasoning operation (3): utilize the steam obtained by heating described purificant (b) described cleaned material to be carried out to the operation of vapour seasoning.

In dehydration procedure (1), use dehydrating agent to be not particularly limited the method that cleaned material is dewatered, the methods such as such as ultrasonic wave, shake, jet flow and circulation can be enumerated.In dehydration procedure (1), from the viewpoint of further improving dehydration property, preferably the physical methods such as dipping, shake, jet flow, ultrasonic wave, spray are combined.

In rinsing process (2), preferably purificant (b) heated and produce steam, being used as purificant (b) by by cooling obtained concentrate to this steam.When particularly using purificant (b) continuously in the dewatering of present embodiment, the concentrate that preferred utilization produces steam and obtains.In rinsing process (2), rinsability from the viewpoint of improving further, preferably the physical methods such as dipping, shake, jet flow, ultrasonic wave, spray are combined.In addition, rinsability from the viewpoint of improving further, more preferably purificant (b) is not in fact containing water.

In vapour seasoning operation (3), utilizing after above-mentioned dehydrating agent (a) dewaters to the water being attached to cleaned material, the steam produced by heating purificant (b) is at least used to carry out vapour seasoning.Such as, can use and regulation liquid be heated and the steam obtained, carry out vapour seasoning.Specifically, heating can be carried out to carry out vapour seasoning to concentrate described later etc., also can carry out heating to carry out vapour seasoning to the mixed liquor containing liquid of more than two kinds.

When carrying out spray rinsing, the pressure that spues of liquid is not particularly limited, from the aspect of dehydration property and the balance on the impact of cleaned material material, is preferably 1 × 10 ³~ 2 × 10 ⁶pa, be more preferably 1 × 10 ⁴~ 1 × 10 ⁶pa.The dewatering of present embodiment is the method at least using above-mentioned dehydrating agent (a), and its dehydration property and drying property are excellent and also few on the impact of cleaned material material, are suitable.

The dewatering of present embodiment preferably has following operation further:

The dehydrating agent (a) of water is had to heat to dissolving in by dewatering, thus by the operation removed at least partially of water contained in described dehydrating agent (a); And

The dehydrating agent (a) of water is eliminated, to the operation that cleaned material is dewatered described in using.

In the dehydrating agent (a) used in dehydration, dissolve in the moisture etc. having and be attached to cleaned material.Making because dehydrating agent (a) has by improving liquid temperature the character that the solubility of water reduces, if thus carry out heating to dehydrating agent (a), liquid temperature being improved, then can reduce saturation moisture concentration.Its result, can be separated the water be added in dehydrating agent (a) with dehydrating agent (a).Dehydrating agent (a) through process like this can give play to excellent dehydrating effect again, can recycle.

The dehydrating agent (a) of recycling can be used in combination with new dehydrating agent (a).Such as, the dehydrating agent (a) eliminating water described in above-mentioned use can carry out with the form of above-mentioned (1) dehydration procedure the operation that cleaned material is dewatered.

For the degree of the liquid temperature of raising dehydrating agent (a), as long as be just not particularly limited without detriment to scope separatory, but be preferably increased to the temperature of higher than the liquid temperature of drench pit more than 15 DEG C.By improving the temperature of paramount more than 15 DEG C, excellent water separable performance can be obtained.From the viewpoint of the dewatering maintaining dehydrating agent, be more preferably increased to the temperature of higher than the liquid temperature of drench pit more than 25 DEG C.

Be not particularly limited by the method for water contained in dehydrating agent (a) removing; known method can be used, the methods such as such as standing separation, the absorption removing based on dehydrating agent, glass fibres etc. such as molecular sieve, ion exchange resin (using after dry), the UF membrane based on coarse film etc. can be enumerated.Among these, from the viewpoint of economy and the aspect of separating power, preferred standing separation.

To dissolved in by rinsing have dehydrating agent (a) purificant (b) in add water, thus described dehydrating agent (a) contained in described purificant (b) is extracted in described water is separated, the operation of the parting liquid (c) that obtains dewatering;

In the purificant (b) used in rinsing process, bring a large amount of dehydrating agents (a) into.By adding water in this purificant (b), the dehydrating agent (a) dissolved in in purificant (b) can be separated with purificant (b).Thereby, it is possible to the rinsing performance of the excellence of long term maintenance purificant (b).

For the addition of the water added in order to purificant (b) is separated with dehydrating agent (a), as long as be just not particularly limited without detriment to scope separatory, but the mass ratio containing purificant (the b)/water of dehydrating agent (a) is preferably the scope of 97/3 ~ 50/50.By making the mass ratio of the water in above-mentioned purificant (b)/water be more than 97/3, dehydrating agent separation property can be improved further.By making the mass ratio of the water in above-mentioned purificant (b)/water be less than 50/50, the effect reducing draining can be improved further.

When considering dehydrating agent parting liquid (c) to use as pre-washing agent (ab), in order to composition (a1) concentration in pre-washing agent (ab) is maintained more than finite concentration, the water content to adding during separating and dehydrating agent is needed to control.From this aspect, the scope of the mass ratio of purificant (b)/water is more preferably 95/5 ~ 60/40.

The purificant (b) of dehydrating agent (a) is had to cool to being dissolved in by rinsing, thus being separated at least partially described dehydrating agent (a) contained in described purificant (b), obtain the operation of dehydrating agent parting liquid (c);

In the dewatering of present embodiment, preferably by dehydrating agent parting liquid (c) as pre-washing agent (ab), before rinsing, carry out prewashing.By carrying out prewashing, can the generation that effectively suppresses rinsing bad further when improving of moisture concentration in dehydrating agent (a).

Specifically, in the dewatering of present embodiment, preferably there is following operation further:

To dissolved in by rinsing have dehydrating agent (a) purificant (b) in add water, thus the described dehydrating agent (a) contained by described purificant (b) is extracted in described water, obtain the operation of the pre-washing agent (ab) containing dehydrating agent parting liquid (c);

Use described pre-washing agent (ab), the cleaned material being attached with dehydrating agent (a) is carried out to the operation of prewashing;

As pre-washing agent (ab), as long as the solvent without detriment to high prewashing is just not particularly limited, such as, the constituent of dehydrating agent (a) and/or purificant (b) can be added, above-mentioned substance also can be used as pre-washing agent.More particularly, from the viewpoint of improving prewashing, preferably containing the glycol ethers monoalkyl ethers (a1) contained by dehydrating agent (a).In this case, the kind of composition (a1) contained in dehydrating agent (a) can be identical with the kind of composition (a1) contained in purificant (b), can be different.

By being used as pre-washing agent (ab) by dehydrating agent parting liquid (c), the constant concentration of the composition (a1) in pre-washing agent can be kept when dewatering continuously.Liquid thus without the need to carrying out pre-washing agent exchanges, and can reduce operating cost.

The concentration of composition (a1) in pre-washing agent (ab) is not particularly limited, consider from the aspect that is rinsability, that obtain high drying property improved based on purificant (b) potcher, preferably reduce the concentration of composition (a1) in dehydrating agent (a) further.In addition, from the viewpoint of further to improve the dehydrating agent composition containing dirt composition displacement, obtain higher prewashing, the concentration of the composition (a1) in preferred purificant (b) is higher.

Further, for the concentration of the composition (a1) in pre-washing agent (ab), more preferably less than composition (a1) in dehydrating agent (a) concentration and higher than the concentration of composition (a1) in purificant (b).Specifically, the concentration of the composition (a1) in pre-washing agent (ab) is preferably 1 ~ 40 quality %, is more preferably 5 ~ 30 quality %.

In addition, in pre-washing agent (ab), the concentration of composition (a1) can be the concentration of the centre of the concentration of composition (a1) in dehydrating agent (a) and the concentration of the middle composition (a1) of purificant (b), and can remain constant density.Its result can obtain higher rinsability.

In prewashing operation, for the object improving prewashing, preferably the physical methods such as dipping, spray, ultrasonic wave are combined.When carrying out prewashing by spray, the pressure that spues is preferably 1 × 10 ³~ 2 × 10 ⁶pa, be more preferably 1 × 10 ⁴~ 1 × 10 ⁶pa.On the basis using dehydrating agent (a), the dehydration property of the dewatering of present embodiment and drying property are excellent, also few on the impact of the material of cleaned material, are suitable.

As the method for carrying out prewashing before rinsing with the pre-washing agent containing composition (a), preferably the physical method such as dipping, spray is combined due to can prewashing be improved.

Or, in the dewatering of present embodiment, as another preferred embodiment when carrying out prewashing operation, preferably there is following operation further:

In the purificant (b) used in rinsing process, bring a large amount of dehydrating agents (a) into.By cooling this purificant (b), purificant (b) can be separated with dehydrating agent (a).Thus can the rinsing performance of excellence of long term maintenance purificant (b).

For the degree of the liquid temperature of reduction purificant (b), as long as be just not particularly limited without detriment to scope separatory, but be preferably reduced to the temperature of low more than 15 DEG C of the liquid temperature than distillation tank (2).By being reduced to the temperature of low more than 15 DEG C, excellent dehydrating agent separation property can be obtained.From the viewpoint of the rinsing performance maintaining purificant (b), be more preferably reduced to the temperature of low more than 20 DEG C of the liquid temperature than distillation tank (2).

The method removed by dehydrating agent (a) contained in purificant (b) is not particularly limited; known method can be used, the methods such as such as standing separation, the absorption removing based on dehydrating agent, glass fibres etc. such as molecular sieve, ion exchange resin (using after dry), the UF membrane based on coarse film or diffusion barrier etc. can be enumerated.Among these, from the viewpoint of economy and the aspect of separating power, preferred standing separation.

< dewater unit >

As an example of the preferred embodiment of dewater unit, the dewater unit possessing following formation can be enumerated: use above-mentioned dehydrating agent (a) to carry out the drench pit of the dehydration of cleaned material; Produce purificant, pre-washing agent if desired or both the distillation tank of steam; By in the concentrate of the described steam produced in described distillation tank except the water separating tank anhydrated; Be used in the concentrate eliminating water in described water separating tank, described cleaned material carried out to the potcher of rinsing; And be used in described distillation tank the described steam produced, dry vapour seasoning portion is carried out to the described cleaned material through rinsing.

When using the dehydrating agent (a) of present embodiment to carry out the dehydration of requirement height dehydration level, as preferred dewater unit, can enumerate as lower device: under the state that drench pit is remained on normal temperature, the cleaned material after the cleaning being attached with water is immersed in the drench pit adding dehydrating agent and dewater; Next make the concentrate of the purificant (b) containing the high composition (b1) of vapour pressure be trapped in dipping potcher, cleaned material be impregnated in and wherein carry out rinsing.Thus rinsing is carried out to the dehydrating agent (a) on the surface being attached to cleaned material, make the temperature of cleaned material reduce simultaneously, thus higher vapour seasoning effect can be obtained.

For dewater unit, carrying out dipping rinsing by making the concentrate of purificant (b) be trapped in potcher, can dehydrating agent be prevented to be attached to the surface of cleaned material again while obtaining excellent wash effect.In addition, flood in potcher and can use the concentrate obtained by heating purificant (b).

Fig. 1 is the schematic diagram of an example of the dewater unit of present embodiment.Dewater unit shown in Fig. 1 possesses: use above-mentioned dehydrating agent (a) to carry out the drench pit 1 of the dehydration of cleaned material; Produce the distillation tank 2 of the steam of purificant; By in described distillation tank 2 produce described steam concentrate in except the water separating tank 3 anhydrated; Be used in the concentrate eliminating water in described water separating tank 3, described cleaned material carried out to the potcher 4 of rinsing; And be used in the described steam produced in described distillation tank 2, dry vapour seasoning portion 5 is carried out to the described cleaned material through rinsing.

When dewatering, such as can by cleaned material being joined in special fixture or basket etc., dewatered by the drench pit 1 of dewater unit, potcher 4, vapour seasoning portion 5 successively.

Drench pit 1 possesses cooling tube 6 and ultrasonic wave generating unit 7.Distillation tank 2 possesses heater 10.Water separating tank 3 possesses cooling tube 11.Dehydrating agent (a) is filled in drench pit 1.The liquid temperature of the dehydrating agent pipe 6 that is cooled controls.In the present embodiment, drench pit 1 preferably possesses the temperature control part controlled the liquid temperature of dehydrating agent (a).Temperature control part is not particularly limited, cooling tube as escribed above, heater etc. can be enumerated.

When dewatering in drench pit 1, ultrasonic wave generating unit 7 can be utilized to irradiate ultrasonic wave the water being attached to cleaned material is dewatered.In present embodiment, also physical force can be share to improve dehydrating effect so further.Such physical force is not particularly limited, the known physical force (in the liquid of such as ultrasonic wave, shake, dehydrating agent jet flow etc.) adopted in dewater unit can be used.

In distillation tank 2, fill purificant (b), utilize heater 10 to heat, become steam (the flowing to 16 of reference steam).A part for the steam produced in distillation tank 2 becomes concentrate via the cooling tube 8,9 of potcher 4, delivers in water separating tank 3 through concentrate pipe arrangement 13.In addition, an other part for steam is used for carrying out vapour seasoning in vapour seasoning portion 5.

In water separating tank 3, while utilizing cooling tube 11 to reduce the liquid temperature of concentrate, remove water contained in concentrate.The removing method of water is not particularly limited, can known method be carried out.From the viewpoint of economy and the aspect of separating power; preferred standing separation; in addition, also can by utilizing the absorption removing of dehydrating agent, the glass fibre etc. such as molecular sieve, ion exchange resin (using after dry), utilizing the methods such as the UF membrane of coarse film etc. to remove moisture.These methods can be used alone a kind, also can share two or more.

The concentrate eliminating water is sent in potcher 4 via the concentrate pipe arrangement 14 after water separation.And utilize the ultrasonic wave generating unit 12 of potcher 4 to irradiate ultrasonic wave while use concentrate to carry out rinsing to the dehydrating agent and water that are attached to cleaned material.In the present embodiment, also physical force can be used to improve wash effect so further.Such physical force is not particularly limited, the known physical force (in the liquid of such as ultrasonic wave, shake, dehydrating agent jet flow etc.) adopted in dewater unit can be used.

In vapour seasoning portion 5, use the steam produced in distillation tank 2, drying is carried out to the cleaned material through rinsing.As an example of the drying means in vapour seasoning portion 5, such as, as mentioned above, utilize cooling tube 8, the steam of 9 pairs of purificants (b) carries out condensation, is collected in water separating tank 3, delivers to immediately in potcher 4 after carrying out standing separation.By cleaned material being immersed in concentrate in potcher 4, the dehydrating agent (a), the water dissolving and/or be scattered in dehydrating agent (a) that are attached to cleaned material are removed.

Concentrate is collected in after in water separating tank 3, and the concentrate pipe arrangement 14 after being again separated by water joins in potcher 4, is back in distillation tank 2 after overflowing (the flowing to 15 of reference concentrate).In distillation tank 2, heater via 10 heats, its part or all become steam (with reference to steam flow to 16), via cooling tube 8,9 carry out condensation, again become concentrate, are back in water separating tank 3 through concentrate pipe arrangement 13.So, purificant (b) can recycle, and thus has economy and can maintain excellent dewatering efficiency.

Fill with the steam produced in distillation tank 2 in vapour seasoning portion 5, vapour seasoning can have been carried out to the cleaned material of carrying out rinsing.For the vapour seasoning utilizing vapour seasoning portion 5 to carry out, due in the liquid that steam produces at the surface condensation of cleaned material not containing dirt composition, refine (on the bodyguard げ) drying thus as dehydration procedure is effective.

In the dewater unit of present embodiment, not only utilize dehydrating agent (a) to dewater, and the state of the purificant (b) making vapour pressure high in device is suitably changed to liquid or gas circulates simultaneously.Further, by utilizing potcher 4 and vapour seasoning portion 5 to carry out rinsing and vapour seasoning, the dehydrating agent of the trace be attached in cleaned material can not only be removed, and can be easy and effectively remove water contained by dehydrating agent.Its result, as requiring that the accurate dewatering of higher dehydration level is also suitable.

In the dewater unit shown in Fig. 1, according to its object or purposes, the number of drench pit and/or potcher also can be made to be more than 2 grooves.In this case, consider from improving the aspect of in the end carrying out the drying property the potcher of rinsing, the content of the composition (a1) in purificant (b) is preferably below 0.5 quality %, is more preferably below 0.1 quality %.

Further, also can by arranging the content that heater (not shown) effectively reduces the composition (a1) in steam in potcher 4.By making also can improve rinsability containing composition (a1) in purificant (b), but when carrying out steam purge with the form of final refine rinsing (refine is dry), from the viewpoint of improving drying property, in preferred purificant (b), not excessively contain the composition (a1) that boiling point is high, drying property is low.Thus, heated by the purificant few to the composition of dehydrating agent (a) compared with distillation tank 2, the steam that cleannes are higher can be produced.

Fig. 2 is the schematic diagram of an other example of the dewater unit of present embodiment.For the dewater unit shown in Fig. 2, it possesses the heating tank 17 that heats dehydrating agent (a) further and will dissolve in the isolated separating tank 18 of the water in described dehydrating agent (a) by described dehydrating agent (a) in the dewater unit shown in Fig. 1.

For in the dehydrating agent (a) that dewaters with a large amount of water.By heating this dehydrating agent (a) in heating tank 17, the liquid temperature of dehydrating agent (a) can be improved.Thereby, it is possible to will dissolve in the water in dehydrating agent (a) by precipitation in dehydrating agent (a).Further, carry out standing separation in separating tank 18 after, dehydrating agent (a) is returned in drench pit 1, and isolated water is discharged to outside system.Excellent dewatering can be maintained thus.By controlling the temperature of the dehydrating agent (a) in drench pit 1, can, while having excellent dewatering for a long time, liquid temperature difference be utilized to carry out water separation.

In heating tank 17, for the dehydrating agent (a) utilizing dehydrating agent liquor charging pump 20 to be transported by drench pit 1 via dehydrating agent liquor charging pipe arrangement 19, heater 21 is adopted to heat.The water be added in dehydrating agent (a) can be isolated thus.By controlling heater 21, can control the liquid temperature of dehydrating agent.Then, be delivered in separating tank 18 via the rework solution pipe arrangement 22 after water separation.

In separating tank 18, to dehydrating agent (a) with dissolve in water wherein and carry out standing separation.Rework solution pipe arrangement 23 after separated dehydrating agent is separated by water is back to drench pit 1, and isolated water is discharged to outside system by draining pipe arrangement 24.For the dewater unit of present embodiment, by being discharged to dissolving in continuously outside system to the water in dehydrating agent (a), the dewatering that dehydrating agent (a) is excellent can be maintained.

In the dewater unit shown in Fig. 2, according to its object, purposes, the number of heating tank and/or separating tank can be set to more than 2 grooves.From the aspect of separating rate, preferable separate groove 18 possesses separator-filter.Being not particularly limited the material of separator-filter, can be any one in woven fabric, woven cloth (volume cloth), non-woven fabrics.

The fiber forming separator-filter is not particularly limited, the fiber of the such as Polyester such as PETG, polybutylene terephthalate (PBT) copolymer can be enumerated; The Fypro such as polyhexamethylene adipamide, polycaprolactam; Polyamide-imide fiber, aromatic polyamide fibre, the poly-fiber to polyester ethers such as p-methoxybenzoic acid esters; The fiber of the halogen containing polymers such as polyvinyl chloride, polyvinylidene chloride, polytetrafluoroethylene (PTFE); The polyolefinic fiber such as polypropylene, polyethylene; Various acrylic fibers peacekeeping vinylal fibre; Regenerated cellulose, acetic acid esters; The natural fibers such as cotton, fiber crops, silk, wool.These fibers can be used alone a kind or two or more combinationally used.In addition, the fluorine-type resin etc. utilizing dimethyl polysiloxane and/or have perfluoroalkyl also can be used to have carried out waterproof processing process to these fibers and the material obtained.

For the single fiber diameter of the fiber of formation separator-filter, as long as be just not particularly limited without detriment to dirt scope separatory, preferably based on the fiber of 0.1 ~ 10 μm, be more preferably the fiber of less than 2 μm based on single fiber diameter.Herein " for main body " refer to, relative to the gross weight of fiber forming separator-filter, the gross weight with the fiber of above-mentioned single fiber diameter is more than 50%.When single fiber diameter is below 10 μm, the removability of microdispersed dirt composition and processing speed can become more preferred; When being more than 0.1 μm, can easily obtain.

For the thickness of separator-filter, as long as just not limiting especially without detriment to dirt scope separatory, but be preferably 0.1 ~ 70mm.By making thickness be more than 0.1mm, more preferred separating effect can be obtained, by being below 70mm, to liquid through time the suppression carried out of the pressure loss can become and be more preferably.

Separator-filter can use flat membranaceous, cylindric, the arbitrary form such as helical form, pleated.From the viewpoint for the treatment of effeciency, separator-filter preferably uses with the form of pleated.In addition, separator-filter can by carrying out lamination to use by 1 or many pieces.Logical liquid method is not particularly limited, such as, can adopts any means such as the penetration by liquid based on gravity, the penetration by liquid based on force feed.

For separator-filter, for objects such as enhancings, also the reinforcing agents such as woven wire, plastics or fiber construct can be used.In addition, the prefilter for trapping impurity etc. also can be set before pass into rework solution in separator-filter, such as impurity capture material that is membranaceous, cushion is set.

As separator-filter, commercially available material can be used, particularly preferably there is separator-filter " the EUTEC " (trade mark of the feature of following (A) or (B); Asahi Chemical Industry weave Co., Ltd. manufacture).

(A): utilize based on single fiber diameter be 0.1 ~ 10 μm fiber, voidage be 30 ~ 90%, thickness be 0.1 ~ 70mm and the critical surface tension of fiber surface for 3.5 × 10 ^-2the separator-filter of more than N/m carries out the separator-filter of great drop separate;

(B): fiber, voidage that to utilize based on single fiber diameter be 0.1 ~ 10 μm be 30 ~ 90%, separator-filter that the separator-filter with water proofing property is separated the dirt composition in rework solution.

As the preferred embodiment that can carry out the dewater unit of above-mentioned dewatering, the dewater unit possessing mixing channel further can be enumerated, in this mixing channel, to owing to dissolving in for described rinsing, the described purificant (b) having described dehydrating agent (a) is middle adds water, thus the described dehydrating agent (a) in described purificant (b) is extracted in described water, obtain dehydrating agent parting liquid (c) for using in described rinsing.

Fig. 3 is the schematic diagram of the another example of the dewater unit of present embodiment.For the dewater unit shown in Fig. 3, it possesses further in the dewater unit shown in Fig. 1: extracted by dehydrating agent (a) in described water by adding water in purificant (b), obtains the mixing channel 25 of dehydrating agent parting liquid (c); And by separating tank 32 that described purificant (b) is separated with described dehydrating agent (a).

The purificant (b) of distillation tank 2 is delivered in mixing channel 25 by purificant liquor charging pump 27.In mixing channel 25, feedwater is supplied by water supply pipe arrangement 28.Purificant (b) and dehydrating agent can be extracted in water thus.Its result, can be separated purificant (b) with dehydrating agent (a).Next, purificant (b) is returned in distillation tank 2, and isolated water and the dehydrating agent (a) do not wanted are discharged to outside system by water and dehydrating agent discharge opeing pipe arrangement 31.By the dehydrating agent (a) be accumulated in distillation tank 2 and water are discharged to outside system continuously, can suppress to produce dry vestige etc. when rinsing and vapour seasoning, and can the rinsing performance of long term maintenance excellence.

In mixing channel 25, the purificant (b) transported is mixed with the water supplied by water supply pipe arrangement 28, utilize cooling tube 29 to cool by purificant liquor charging pump 27 by distillation tank 2 through purificant liquor charging pipe arrangement 26.Such as, in purificant (b) containing composition (b1), because composition (b1) has the character that dissolution characteristics significantly changes along with liquid temperature, thus by utilizing cooling tube 29 pairs of purificants (b) to cool, liquid temperature is reduced, the water-soluble of composition (b1) greatly reduces.Its result, the water-soluble of purificant (b) also reduces.Thereby, it is possible to the dehydrating agent (a) be dissolved in purificant (b) is extracted in water.

In mixing channel 25, when being extracted in water by dehydrating agent (a), preferably use physical force.As physical force, as long as be the physical force such as stirring, ultrasonic wave, jet flow, circulation, any method can be used.

In the dewater unit of present embodiment, by the dehydrating agent (a) dissolved in purificant (b) is discharged to outside system continuously, the rinsing performance that purificant (b) is excellent can be maintained, can be suitable in the dehydration of the higher dehydration level of requirement.

In the dewater unit shown in Fig. 3, according to its object, purposes, the number of mixing channel can be set to more than 2 grooves.Further, preferably separator-filter is set after mixing channel because separating rate can accelerate.

Fig. 4 is the schematic diagram of an example again of the dewater unit of present embodiment.For the dewater unit shown in Fig. 4, it possesses further in the dewater unit shown in Fig. 1: by having the described purificant (b) of described dehydrating agent (a) to cool and being separated at least partially the described dehydrating agent (a) in described purificant (b) to dissolving in, obtain the cooling bath 33 of dehydrating agent parting liquid (c) for using in rinsing; And to the separating tank 34 that described purificant (b) is separated with dehydrating agent (a).

By cooling purificant (b) in cooling bath 33, the saturated concentration of ordinary dissolution of purificant reduces, and thus purificant (b) can be separated with dehydrating agent (a).Next, returning through purificant delivers in separating tank 34 with pipe arrangement 30a, carry out standing separation in separating tank 34 after, dehydrating agent parting liquid (c) returns through purificant and is back to distillation tank 2 with pipe arrangement 30b, meanwhile, the isolated parting liquid containing dehydrating agent (a) is discharged to outside system by water and dehydrating agent discharge opeing pipe arrangement 31.By the dehydrating agent (a) be accumulated in distillation tank 2 is discharged to outside system continuously, can suppress to produce dry vestige etc. when rinsing and vapour seasoning, and can the rinsing performance of long term maintenance excellence.

In cooling bath 33, for the purificant (b) utilizing purificant liquor charging pump 27 to be transported by distillation tank 2 via purificant liquor charging pipe arrangement 26, cooling tube 37 is adopted to cool.Such as, when purificant (b) is containing composition (b1), because composition (b1) has the character that dissolution characteristics significantly changes along with liquid temperature, thus by utilizing cooling tube 37 pairs of purificants (b) to carry out cooling, liquid temperature is reduced, dehydrating agent dissolubility greatly reduces.Thereby, it is possible to effectively the dehydrating agent (a) be dissolved in purificant (b) is isolated.

On the other hand, the purificant of the purificant (b) containing dehydrating agent (a) after dehydrating agent is separated through cooling returns and is delivered in separating tank 34 with pipe arrangement 30a.In separating tank 34, standing separation is carried out to purificant (b) and dehydrating agent (a).Dehydrating agent parting liquid (c) returns through purificant and is back in distillation tank 2 with pipe arrangement 30b, and the parting liquid containing dehydrating agent (a) is discharged to outside system by water and dehydrating agent discharge opeing pipe arrangement 31.

In cooling bath 33, when being separated dehydrating agent (a), preferably use physical force.As physical force, as long as be the physical force such as stirring, ultrasonic wave, jet flow, circulation, any method can be used.

In the dewater unit of present embodiment, by purificant (b) and dehydrating agent (a) are discharged to outside system continuously, the rinsing performance that purificant (b) is excellent can be maintained, can be suitable in the dehydration of the higher dehydration level of requirement.

In the dewater unit shown in Fig. 4, according to its object, purposes, also the number of cooling bath and/or separating tank can be set to more than 2 grooves.Further, preferably separator-filter is set after cooling bath because separating rate can accelerate.

Fig. 5 is the schematic diagram of another example again of the dewater unit of present embodiment.In the present embodiment, the dewater unit possessing prewash tank further can be used, share above-mentioned pre-washing agent and dewater.Dewater unit shown in Fig. 5 possesses:

Use the drench pit 1 that above-mentioned dehydrating agent (a) is dewatered to cleaned material;

Produce the distillation tank 2 of purificant (b), pre-washing agent (ab) or the steam of both;

At least be used in the described steam produced in described distillation tank 2 and dry vapour seasoning portion 5 is carried out to cleaned material;

Described steam is made to cool the cooling end (cooling tube 8,9) becoming concentrate;

By the water separating tank 3 being separated water outlet in described concentrate;

Use the described concentrate being separated water, described cleaned material is carried out to the potcher 4 of rinsing;

To dissolving in the heating tank 17 having the described dehydrating agent (a) of water to heat;

The first separating tank 18 of water outlet is separated by described dehydrating agent (a);

By to dissolve in have described dehydrating agent (a) described purificant (b) in add water and being extracted at least partially in water of the described dehydrating agent (a) in described purificant (b) removed, obtain the mixing channel 25 of the pre-washing agent (ab) containing obtained dehydrating agent parting liquid (c);

By described purificant (b) and dehydrating agent (a) by the second separating tank 32 isolated in described purificant (b);

Described pre-washing agent (ab) is utilized to carry out the prewash tank 40 of prewashing to described cleaned material; And

Described pre-washing agent (ab) is carried out to the liquor charging portion (pre-washing agent circulation pipe arrangement 45) of liquor charging between described distillation tank 2 and described prewash tank 40.

In the dehydration of reality, cleaned material can be added in special fixture or basket etc., in dewater unit successively by drench pit 1, prewash tank 40, potcher 4, vapour seasoning portion 5 while complete dehydration.

In drench pit 1, under the state utilizing the liquid temperature of cooling tube 6 pairs of dehydrating agents to control, produce ultrasonic wave by ultrasonic wave generating unit 7 while use described dehydrating agent (a) to carry out dehydration removal to the water being attached to cleaned material.Physical force used when removing as dehydration, is not limited to ultrasonic wave, if for shake or dehydrating agent liquid in the physical force that adopts in dewaterer such as jet flow just can use arbitrary method.The cooling means used in drench pit 1 is not particularly limited, known method can be adopted.Such as can enumerate the water-cooled, Air flow etc. that use cooling tube.

In prewash tank 40, can use processing in mixing channel 25 dehydrating agent parting liquid (c) obtained as pre-washing agent (ab).Prewash tank 40 possesses ultrasonic wave generating unit 41, uses ultrasonic wave to carry out prewashing to the dehydrating agent (a) and the water dissolved in wherein that are attached to cleaned material.In mixing channel 25, isolated dehydrating agent parting liquid (c) is back in distillation tank 2, be delivered to after in prewash tank 40 via pre-washing agent circulation pipe arrangement 45 by prewash tank circulation pump 44, its part is overflowed, and to be back in distillation tank 2 (reference concentrate and pre-washing agent flow to 43).As physical force during prewashing, the known physical force adopted in the dewaterer such as jet flow in the liquid of shake, ultrasonic wave and dehydrating agent can be used.

In potcher 4, becoming the purificant (b) of steam for utilizing the heater 10 of distillation tank 2 to carry out heating, utilizing cooling tube 8 and 9 to cool, making concentrate, being delivered in water separating tank 3 via concentrate pipe arrangement 13.In water separating tank 3, while utilizing cooling tube 11 to reduce the liquid temperature of concentrate, removing moisture.Then, use the concentrate pipe arrangement 14 after via water separation to be back in potcher 4, to eliminate moisture concentrate, rinsing removal is carried out to the dehydrating agent (a) and water being attached to cleaned material.Now, the ultrasonic wave produced by ultrasonic wave generating unit 12 can be share and carry out rinsing.As physical force, as long as the physical force adopted in dewater unit so far for jet flow etc. in the liquid of ultrasonic wave, shake, dehydrating agent, any method can be used.

In vapour seasoning portion 5, utilize cooling tube 8, the steam of purificant (b) and/or pre-washing agent (ab) cools by 9, makes concentrate, is collected into after in water separating tank 3, delivers in potcher 4 through concentrate pipe arrangement 13.In potcher 4, carrying out rinsing by cleaned material being immersed in concentrate, removing the pre-washing agent (ab) being attached to cleaned material.Then, a part for the concentrate of potcher 4 is overflowed, and flow to (the flowing to 42 of reference concentrate) in prewash tank 40, overflows further, to be back in distillation tank 2 (with reference to concentrate and pre-washing agent flow to 43), to be subject to the heating of heater 10.Then, its part or all become steam (with reference to steam flow to 16), through cooling tube 8, after 9 condensations, again delivered in water separating tank 3 by concentrate pipe arrangement 13.

Be full of by the steam produced in distillation tank 2 in vapour seasoning portion 5, for the vapour seasoning of carrying out in vapour seasoning portion 5, due in the liquid that steam produces at cleaned material surface condensation not containing dirt composition, be thus effective as the refine drying that dehydration procedure is last.

In heating tank 17, for the dehydrating agent (a) utilizing dehydrating agent liquor charging pump 20 to be transported through dehydrating agent liquor charging pipe arrangement 19 by drench pit 1, heater 21 is adopted to heat.The elutriation be added in dehydrating agent (a) is made to go out thus.And deliver in the first separating tank 18 via the rework solution pipe arrangement 22 after water is separated.

In the first separating tank 18, will dissolve in the water in dehydrating agent (a) by standing separation in dehydrating agent (a).Returning after isolated dehydrating agent (a) is separated by water is back in drench pit 1 with pipe arrangement 23.On the other hand, isolated water is discharged to outside system by draining pipe arrangement 24.

In mixing channel 25, the pre-washing agent (ab) transported is mixed with the water supplied by water supply pipe arrangement 28, utilize cooling tube 29 to cool by pre-washing agent liquor charging pump 36 by distillation tank 2 through pre-washing agent liquor charging pipe arrangement 35.Then return via pre-washing agent and deliver in the second separating tank 32 with pipe arrangement 38a.The dehydrating agent (a) be dissolved in pre-washing agent (ab) can be extracted in water thus and be separated.

In the second separating tank 32, by pre-washing agent (ab) and dehydrating agent (a) standing separation, obtain dehydrating agent parting liquid (c).Dehydrating agent parting liquid (c) is returned by pre-washing agent and is back in distillation tank 2 with pipe arrangement 38b, be back in heating tank 17 by the isolated parting liquid containing dehydrating agent (a) by dehydrating agent discharge opeing pipe arrangement 39, the composition as dehydrating agent (a) recycles simultaneously.

As the liquor charging portion for dehydrating agent parting liquid (c) of process in mixing channel 25 being carried out between distillation tank 2 and prewash tank 40 liquor charging, employing prewash tank circulation pump 44, but being not particularly limited, can the known formations such as pump be adopted.

Fig. 6 is the schematic diagram of the example more again of the dewater unit of present embodiment.Dewater unit shown in Fig. 6 possesses:

The described steam produced in described distillation tank 2 is at least used to carry out dry vapour seasoning portion 5 to cleaned material;

Use the described concentrate being separated water, the described cleaned material being attached with dehydrating agent (a) is carried out to the potcher 4 of rinsing;

By the first separating tank 18 being separated water outlet in the described dehydrating agent (a) of carrying out heating in described heating tank;

Cool dissolving in the described pre-washing agent (ab) having described dehydrating agent (a), thus being separated at least partially the described dehydrating agent (a) in described pre-washing agent (ab), obtain the cooling bath 33 of the pre-washing agent (ab) containing obtained dehydrating agent parting liquid (c);

By the second separating tank 34 isolating dehydrating agent (a) in the pre-washing agent (ab) having carried out described cooling;

For the dewater unit shown in Fig. 6, not supplying new water, liquid is circulated in cooling bath 33, is at least different in this.In the dewater unit shown in Fig. 5, fetch carry out lock out operation by carrying out water extraction in mixing channel 25; In the dewater unit shown in Fig. 6, by cooling liquid in cooling bath 33, saturation solubility is controlled, carry out lock out operation thus.

In drench pit 1, under the state utilizing the liquid temperature of cooling tube 6 pairs of dehydrating agents to control, produce ultrasonic wave by ultrasonic wave generating unit 7 while use above-mentioned dehydrating agent (a) to carry out dehydration removal to the water being attached to cleaned material.Physical force used when removing as dehydration, is not limited to ultrasonic wave, if for shake or dehydrating agent liquid in the physical force that adopts in dewaterer such as jet flow just can use arbitrary method.The cooling means used in cooling bath 33 is not particularly limited, known method can be adopted.Such as can enumerate the water-cooled, Air flow etc. that use cooling tube.Thus the dehydrating agent (a) be dissolved in purificant (b) is separated.

On the other hand, pre-washing agent (ab) returns via pre-washing agent and is delivered in the second separating tank 34 with pipe arrangement 38a.By pre-washing agent (ab) and dehydrating agent (a) standing separation in the second separating tank 34.Dehydrating agent parting liquid (c) returns via pre-washing agent and is back in distillation tank 2 with pipe arrangement 38b, and the parting liquid containing dehydrating agent (a) is back in heating tank 17 by dehydrating agent discharge opeing pipe arrangement 39.The pre-washing agent of dehydrating agent parting liquid (c) after dehydrating agent is separated returns and is back in distillation tank 2 with pipe arrangement 38b, be delivered to after in prewash tank 40 via pre-washing agent circulation pipe arrangement 45 further by prewash tank circulation pump 44, its part is overflowed, and to flow back in distillation tank 2 (reference concentrate and pre-washing agent flow to 43).In prewash tank 40, dehydrating agent parting liquid (c) is utilized as pre-washing agent (ab).Use the ultrasonic wave that produced by ultrasonic wave generating unit 41 while to being attached to the dehydrating agent of cleaned material and dissolving in water wherein and carry out prewashing.

In potcher 4, in distillation tank 2, utilize heater 10 pairs of pre-washing agents (ab) to heat, utilize cooling tube 8,9 pairs of steams carry out condensation, are delivered in water separating tank 3 through concentrate pipe arrangement 13.In water separating tank 3, cooling tube 11 is utilized to reduce the liquid temperature of concentrate, removing moisture.The concentrate eliminating moisture is back in potcher 4 via the concentrate pipe arrangement 14 after water separation, while use by the ultrasonic wave produced in ultrasonic wave generating unit 12, rinsing is carried out to the pre-washing agent containing the dehydrating agent and water that are attached to cleaned material and removes.As physical force, as long as the physical force adopted in dewaterer so far for jet flow etc. in the liquid of ultrasonic wave, shake, dehydrating agent, any method can be used.

In vapour seasoning portion 5, utilize cooling tube 8,9 by the steam condensing of pre-washing agent (ab), is collected into after in water separating tank 3, delivers in potcher 4.In potcher 4, carrying out rinsing by cleaned material being immersed in concentrate, removing the dehydrating agent (a) that is attached to cleaned material and containing the pre-washing agent brought into the water in dehydrating agent (a).Then, a part for the concentrate of potcher 4 is overflowed, and flow to (the flowing to 42 of reference concentrate) in prewash tank 40, overflows further, to be back in distillation tank 2 (with reference to concentrate and pre-washing agent flow to 43), to be subject to the heating of heater 10.Then, its part or all become steam (with reference to steam flow to 16), through cooling tube 8, after 9 condensations, again delivered in water separating tank 3 by concentrate pipe arrangement 13.

Be full of by the steam produced in distillation tank 2 in vapour seasoning portion 5, for the vapour seasoning of carrying out in vapour seasoning portion 5, due in the liquid that steam produces at cleaned material surface condensation not containing dirt composition, be thus effective especially as the refine drying that dehydration procedure is last.

In heating tank 17, for the dehydrating agent (a) utilizing dehydrating agent liquor charging pump 20 to be transported through dehydrating agent liquor charging pipe arrangement 19 by drench pit 1, heater 21 is adopted to heat.The elutriation dissolved in in dehydrating agent (a) is made to go out thus.And deliver in the first separating tank 18 via the rework solution pipe arrangement 22 after water is separated.

In cooling bath 33, for the pre-washing agent (ab) utilizing pre-washing agent liquor charging pump 36 to be transported by distillation tank 2 via pre-washing agent liquor charging pipe arrangement 35, cooling tube 37 is adopted to cool.Thus, the dehydrating agent (a) being dissolved in pre-washing agent (ab) is separated by pre-washing agent (ab).Isolated dehydrating agent parting liquid (c) is returned by pre-washing agent and is delivered in the second separating tank 34 with pipe arrangement 38a.

In the second separating tank 34, by pre-washing agent (ab) and dehydrating agent (a) standing separation, obtain dehydrating agent parting liquid (c).Isolated dehydrating agent parting liquid (c) is returned by pre-washing agent and is back in distillation tank 2 with pipe arrangement 38b, composition as pre-washing agent recycles, the isolated parting liquid containing dehydrating agent (a) is back to heating tank 17 by dehydrating agent discharge opeing pipe arrangement 39, and the composition as dehydrating agent (a) recycles.

As the liquor charging portion for dehydrating agent parting liquid (c) being carried out between distillation tank 2 and prewash tank 40 liquor charging, employing prewash tank circulation pump 44, but being not particularly limited, can the known formations such as pump be adopted.

In the dewater unit of present embodiment, before rinsing with dehydrating agent parting liquid (c) for pre-washing agent (ab), by carrying out dipping rinsing, reduce dehydrating agent and be dissolved in the residual quantity of water on cleaned material surface in dehydrating agent, thus the life-span of dehydrating agent can be improved tremendously; Further, by improving rinsing and vapour seasoning effect, higher dewatering can be obtained.Further, water separation circuit (heating tank 17) is back to by making the parting liquid containing dehydrating agent (a), the dehydrating agent (a) taken out of for being attached to cleaned material by drench pit recycles, make the consumption of dehydrating agent significantly cut down thus, thus can operating cost be reduced.

The dehydrating agent of present embodiment, use the dewatering of this dehydrating agent and dewater unit can be suitable for the dehydration of precision instrument, optical instrument, electronic instrument and common metal parts etc.Be particularly suitable for the dehydration of the glasswares such as the optical lens of requirement high drying property or hard disk drive.

Embodiment

Below by embodiment, the present invention is specifically described further, but the present invention is not by any restriction of following examples.In addition, the various physical property such as dehydrating agent carries out measuring, evaluating as follows.

[embodiment 1 ~ 5 and comparative example 1 ~ 16]

(1) water separable performance test

In 30mL sample cell, add 14g water and 14g composition (a1), with hand dynamic 1 minute, sample cell is flooded 30 minutes being set in the Water Tank with Temp.-controlled of 25 DEG C, its uniform dissolution of visual confirmation.Transfer them in the Water Tank with Temp.-controlled being set in 55 DEG C and flood after 30 minutes, take out, outward appearance is observed.During water separable performance is evaluated, the visual phase-separated state of outward appearance is evaluated.Evaluate based on following benchmark.

" ◎ ": 25 DEG C of uniform dissolution, be separated at 55 DEG C.Further, in water layer, composition (a1) concentration is below 20 quality %.

"○": 25 DEG C of uniform dissolution, be separated at 55 DEG C.

"×": in arbitrary temperature all uniform dissolution of 25 DEG C and 55 DEG C.

Embodiment 1 ~ 5

The each dehydrating agent recorded for table 1 carries out water separable performance test, and result is compiled in table 1.When liquid temperature is brought up to 55 DEG C by 25 DEG C, being separated all has appearred in the glycol ethers (a1) be engaged in dehydrating agent.Confirm thus, can the water be added in dehydrating agent (a) be separated.Particularly in example 4, the concentration confirming the glycol ethers (a1) in water layer is below 20 quality %, and drainage load is few.

Comparative example 1 ~ 16

The solvent recorded for table 1 carries out the evaluation test identical with embodiment.Result is compiled in table 1.For the glycol ethers of carrying out testing, liquid temperature is brought up to 55 DEG C also do not occur being separated even if confirm, the separation of water cannot be carried out.

[table 1]

[embodiment 6 ~ 26]

(2) dehydration property test

With each dehydrating agent, stainless steel metal silk screen is dewatered, utilize following time-and-motion study dehydration property.

By 30 object stainless steel metal silk screen (27cm ²) be immersed in distilled water, apply 30 seconds ultrasonic waves (28kHz), make sample.The dehydrating agent 100mL of 25 DEG C is utilized to carry out 1 minute supersonic dewatering (28kHz) to it, utilize 1H, 1H, 1H, 3H, 3H-perfluorinated butane (trade name: Solkane365mfc, SOLVAY Co., Ltd. of Japan manufactures) and methyl perfluoro butyl ether, mixture (the trade name: Novec HFE-7100 of methyl perfluoro isobutyl ether, Sumitomo 3M society manufacture) mixture (Solkane365mfc/Novec HFE-7100=88/12 quality %) carry out rinsing and vapour seasoning after, absolute methanol 30mL is utilized to carry out the extraction of moisture, determination of moisture is carried out by Karl_Fischer method.Evaluate based on following benchmark.

"○": moisture entrapment amount is less than 10mg/ sheet

"×": moisture entrapment amount is more than or equal to 10mg/ sheet

Dehydration procedure: liquid temperature 20 DEG C, ultrasonic wave 28kHz, 1 minute

Rinsing process 1: liquid temperature 20 DEG C, ultrasonic wave 28kHz, 1 minute

Rinsing process 2: liquid temperature 20 DEG C, ultrasonic wave 28kHz, 1 minute

Vapour seasoning: 1 minute

Embodiment 6 ~ 26

The each dehydrating agent (a) recorded for table 2 carries out dehydration property test, and result is compiled in table 2.For the dehydrating agent (a) adding certain water gaging (a2) in glycol ethers (a1), moisture entrapment amount is all less than 10mg/ sheet, confirms and has equal excellent dewatering with the isopropyl alcohol shown in reference example 1.

[table 2]

[embodiment 27 ~ 31]

(3) glycol ethers separation property test

By composition (a1) and composition (b1) in certain proportion ((a1)/(b1)=50/50 quality %) mix in 30mL sample cell, after making the homogeneous solution of uniform dissolution, by each homogeneous solution and composition (a2) in certain proportion (=65/35 quality %) mix, then with hand dynamic 1 minute.After leaving standstill 30 minutes at 25 DEG C, take out and observe outward appearance.For glycol ethers separation property, the visual phase-separated state of outward appearance is evaluated.Evaluate based on following benchmark.

" ◎ ": be separated.And then composition (a1) concentration contained in composition (b1) is more than 5 quality %.

"○": be separated.

"×": do not occur being separated.

Composition (b1): 1H, 1H, 1H, 3H, 3H-perfluorinated butane (trade name: Solkane365mfc, Japanese SOLVAY Co., Ltd. manufacture)

Embodiment 27,28,31

The each glycol ethers recorded for table 3 carries out the test of glycol ethers separation property, and result is compiled in table 3.Have in composition (a1) and the solution of composition (b1) to uniform dissolution and add composition (a2), being separated appears in result, confirms and the composition (a1) dissolved in in composition (b 1) can be isolated.

Embodiment 29,30

The each composition (a1) recorded for table 3 carries out the test of glycol ethers separation property, and result is compiled in table 3.Have in composition (a1) and the solution of composition (b1) to uniform dissolution and add composition (a2), be separated, confirm and the composition (a1) dissolved in in composition (b1) can be isolated.Further, the concentration confirming composition (a1) contained in composition (b1) is more than 5 quality %, confirms that it is as the suitable composition of pre-washing agent.

[table 3]

[embodiment 32 ~ 71]

(4) prewashing test

After glass slide is flooded 30 seconds in 100mL dehydrating agent, flood 5 minutes in isolated lower floor (g) liquid in the embodiment 30 of (3) dehydrating agent separation test, observe rinsability.Prewashing is evaluated, exposes to glass slide by oblique for the light of projector, evaluated by the surface state of the visual glass slide of outward appearance.Evaluate based on following benchmark.

" ◎ ": glass slide surface remaining without dehydrating agent

"○": remaining of the surperficial slightly dehydrating agent of glass slide

"×": glass slide surface remains dehydrating agent in drops

Embodiment 32 ~ 52,56,60,64,68

The each dehydrating agent recorded for table 4 carries out the test of dehydrating agent separation property, and result is compiled in table 4.Confirming by utilizing dehydrating agent parting liquid (c) of embodiment 31 to carry out prewashing, abundant rinsing can be carried out to the dehydrating agent being attached to glass slide surface.

Embodiment 53 ~ 55,57 ~ 59,61 ~ 63,65 ~ 67,69 ~ 71

The each dehydrating agent (a) recorded for table 4 carries out the test of dehydrating agent separation property.Result is compiled in table 4.Even confirm the purificant not containing composition (a2), also substantially rinsing can be carried out to the dehydrating agent being attached to glass slide surface.

[table 4]

[embodiment 72]

(5) dehydrating agent separation property test

After by composition (a1), water (a2) and composition (b1), (composition (a1)/water (a2)/composition (b1)=52/3/45 quality %) mixes in 30mL sample cell in certain proportion, with hand dynamic 1 minute.After leaving standstill 30 minutes at 15 DEG C, take out, outward appearance is once observed.Further with after hand dynamic 1 minute, leave standstill 30 minutes at 40 DEG C, outward appearance is observed again.Dehydrating agent separation property is evaluated by the visual phase-separated state of outward appearance.Evaluate based on following benchmark.

"○": occur being separated at 15 DEG C, is separated and uniform dissolution 40 DEG C of nothings.

"×": all do not occur being separated under any liquid temperature of 15 DEG C and 40 DEG C.

Composition (a1): diethylene glycol list benzyl oxide

Embodiment 72

Utilize with the liquid of the ratio of above-mentioned record mixing, carry out the test of dehydrating agent separation property, result gathers as follows.

Separation property: zero

For diethylene glycol list benzyl oxide, in 3 component system of composition (a1), composition (a2) and composition (b1), being occurred by the change of liquid temperature being separated, confirming the separation property without the need to adding water to carry out the excellence be separated.

[embodiment 73 ~ 83 and comparative example 17]

(5) flash(ing) test

Based on JIS K 2265, carry out flashing test with Cleveland open type.Evaluate based on following benchmark.

" ◎ ": without flash-point

"○": flash-point is more than 45 DEG C

"×": flash-point is less than 45 DEG C

Embodiment 73 ~ 78

The composition utilizing table 5 to record mixes each composition, obtains object dehydrating agent.Carry out flash(ing) test for each dehydrating agent, result is compiled in table 5.Confirm by adding water (a2) in glycol ethers, flash-point is eliminated.

Embodiment 79 ~ 83

The dehydrating agent utilizing table 5 to record carries out flash(ing) test.Result is compiled in table 5.The flash-point carrying out the dehydrating agent tested is all 45 DEG C, confirms fire hazard low.

Comparative example 17

The solvent recorded for table 5 carries out flash(ing) test in the same manner as embodiment.Result is compiled in table 5.

Its result, has confirmed flash-point.

[table 5]

The Japanese patent application (Japanese Patent Application 2009-111408) that the application submitted to Japan Office based on April 30th, 2009, introduces this description with the form of reference by its content.

Industrial applicibility

The technology that the present invention removes as the dehydration at precision instrument, optical instrument, electronic instrument and common metal parts etc. the moisture being attached to cleaned material surface is afterwards suitable.

Symbol description

1 ... drench pit, 2 ... distillation tank, 3 ... water separating tank, 4 ... potcher, 5 ... vapour seasoning portion, 6,8,9,11,29,37 ... cooling tube, 7,12,41 ... ultrasonic wave generating unit, 10,21 ... heater, 13 ... concentrate pipe arrangement, 14 ... concentrate pipe arrangement after water is separated, 15 ... the flow direction of concentrate, 16 ... the flow direction of steam, 17 ... heating tank, 18,32,34 ... separating tank, 19 ... dehydrating agent liquor charging pipe arrangement, 20 ... dehydrating agent liquor charging pump, 22,23 ... rework solution pipe arrangement after water is separated, 24 ... draining pipe arrangement, 25 ... mixing channel, 26 ... purificant liquor charging pipe arrangement, 27 ... purificant liquor charging pump, 28 ... water supply pipe arrangement, 30,30a, 30b ... purificant returns with pipe arrangement, 31 ... water and dehydrating agent discharge opeing pipe arrangement, 33 ... cooling bath, 35 ... pre-washing agent liquor charging pipe arrangement, 36 ... pre-washing agent liquor charging pump, 38a, 38b ... pre-washing agent returns with pipe arrangement, 39 ... dehydrating agent discharge opeing pipe arrangement, 40 ... prewash tank, 42 ... the flow direction of concentrate, 43 ... the flow direction of concentrate and pre-washing agent, 44 ... prewash tank circulation pump, 45 ... pre-washing agent circulation pipe arrangement

Claims

1. a dehydrating agent a, it contains the composition a1 glycol ethers shown in following formula (1) of 40 quality % ~ 95 quality % and the composition a2 water of 60 quality % ~ 5 quality %:

R ¹O―(R ²O) _n―H (1)

In formula (1), R ¹represent that carbon number is alkyl, the carbon number alkenyl that is 6 or 7, carbon number be 6 or 7 cycloalkyl, phenyl or benzyl, the R of 6 or 7 ²represent that carbon number is the alkylidene of 2 or 3, n represents the integer of 1 ~ 3.

2. dehydrating agent a as claimed in claim 1, wherein, described composition a1 is diethylene glycol monohexyl ether or diethylene glycol list benzyl oxide.

3. dehydrating agent a as claimed in claim 1, wherein, described composition a1 is diethylene glycol list benzyl oxide.

4. dehydrating agent a as claimed in claim 1, wherein, this dehydrating agent a contains 40 quality % ~ 90 quality % and meets composition a2 water described in the described composition a1 of the condition of following (i) and (ii) and 60 quality % ~ 10 quality %,

I when described composition a1 carries out mixing with the ratio of mass ratio 1:1 with described composition a2 by (), if leave standstill at 10 ~ 30 DEG C, uniform dissolution, and, if leave standstill at 40 ~ 70 DEG C, be separated into 2 layers of upper strata d and lower floor e;

(ii) when described composition a1, described composition a2 being carried out mixing with the ratio of mass ratio 52:3:45 with composition b1, if leave standstill at 35 DEG C, uniform dissolution, and, if leave standstill at 15 DEG C, be separated into 2 layers of upper strata f and lower floor g, described composition b1 is 1.33 × 10 the vapour pressure of 20 DEG C ³the chlorine-free fluorine compounds of more than Pa.

5. the dehydrating agent a as described in any one of Claims 1 to 4, wherein, this dehydrating agent a is same composition with the lower floor e recorded in following condition (i):

I when described composition a1 carries out mixing with the ratio of mass ratio 1:1 with described composition a2 by (), if leave standstill at 10 ~ 30 DEG C, uniform dissolution, and, if leave standstill at 40 ~ 70 DEG C, be separated into 2 layers of upper strata d and lower floor e.

6. a dewatering, it has following operation:

(1) the dehydrating agent a described in any one of claim 1 ~ 5 is used, to the operation that cleaned material is dewatered;

(2) use containing the purificant b of composition b1, the cleaned material being attached with described dehydrating agent a is carried out to the operation of rinsing, described composition b1 is 1.33 × 10 the vapour pressure of 20 DEG C ³the chlorine-free fluorine compounds of more than Pa; And

(3) at least using the steam obtained by heating purificant b, described cleaned material being carried out to the operation of vapour seasoning.

7. dewatering as claimed in claim 6, wherein, the method has following operation further:

The described dehydrating agent a of water is had to heat to being dissolved in by described dehydration, thus by the operation removed at least partially of water contained in described dehydrating agent a; And

The dehydrating agent a of water is eliminated, to the operation that described cleaned material is dewatered described in reusing.

8. dewatering as claimed in claims 6 or 7, wherein, the method has following operation further:

Add water to dissolving in have in the purificant b of dehydrating agent a by described rinsing, thus described dehydrating agent a contained in described purificant b is extracted in described water is separated, obtain the operation of dehydrating agent parting liquid c;

Described dehydrating agent parting liquid c is heated, obtains the operation of the concentrate of described dehydrating agent parting liquid c; And

9. dewatering as claimed in claims 6 or 7, wherein, the method has following operation further:

The purificant b of dehydrating agent a is had to cool to being dissolved in by described rinsing, thus being separated at least partially described dehydrating agent a contained in described purificant b, obtain the operation of dehydrating agent parting liquid c;

10. dewatering as claimed in claims 6 or 7, wherein, the method has following operation further:

Add water to dissolving in have in the purificant b of dehydrating agent a by described rinsing, thus described dehydrating agent a contained in described purificant b is extracted in described water, obtain the operation of the pre-washing agent ab containing dehydrating agent parting liquid c;

Use described pre-washing agent ab, described cleaned material is carried out to the operation of prewashing;

Described pre-washing agent ab is heated, obtains the operation of the concentrate of pre-washing agent ab; And

11. dewaterings as claimed in claims 6 or 7, wherein, the method has following operation further:

After described (2) operation, cooling dissolving in the purificant b having dehydrating agent a, a part of the dehydrating agent a in purificant b being separated, obtaining the operation of the pre-washing agent ab containing dehydrating agent parting liquid c;

Use pre-washing agent ab, the cleaned material being attached with dehydrating agent a is carried out to the operation of prewashing;

Pre-washing agent ab is heated, obtains the operation of the concentrate of pre-washing agent ab; And

Use described concentrate, the cleaned material being attached with dehydrating agent a is carried out to the operation of rinsing.

12. 1 kinds of dewater units, it possesses:

Use the drench pit that the dehydrating agent a described in any one of claim 1 ~ 5 dewaters to cleaned material;

Produce the distillation tank of purificant b, pre-washing agent ab or the steam of both;

13. dewater units as claimed in claim 12, wherein, this device possesses further:

To the heating tank that described dehydrating agent a heats; And

By the separating tank being separated water outlet in described dehydrating agent a.

14. dewater units as described in claim 12 or 13, wherein, this device possesses further:

By adding water in described purificant b, described dehydrating agent a being extracted in described water, obtaining the mixing channel of dehydrating agent parting liquid c; And

The separating tank be separated with described purificant b to the described dehydrating agent a in described purificant b will be dissolved in.

15. dewater units as described in claim 12 or 13, wherein, this device possesses further:

By having the described purificant b of described dehydrating agent a to cool and being separated at least partially the described dehydrating agent a in described purificant b to dissolving in, obtain the cooling bath of the dehydrating agent parting liquid c for using in rinsing; And

To the separating tank that described purificant b is separated with dehydrating agent a.

16. 1 kinds of dewater units, it possesses:

Described steam is made to cool the cooling end becoming concentrate;

To dissolving in the heating tank having the described dehydrating agent a of water to heat;

The first separating tank of water outlet is separated by described dehydrating agent a;

By to dissolve in have described dehydrating agent a described purificant b in add water and being extracted at least partially in water of the described dehydrating agent a in described purificant b removed, obtain the mixing channel of the pre-washing agent ab containing obtained dehydrating agent parting liquid c;

To the second separating tank that described purificant b is separated with dehydrating agent a;

Described pre-washing agent ab is utilized described cleaned material to be carried out to the prewash tank of prewashing; And

Described pre-washing agent ab is carried out to the liquor charging portion of liquor charging between described distillation tank and described prewash tank.

17. 1 kinds of dewater units, it possesses:

Described steam is made to cool the cooling end becoming concentrate;

By the first separating tank being separated water outlet in the described dehydrating agent a heated in described heating tank;

There is the described purificant b of described dehydrating agent a to cool thus being separated at least partially the described dehydrating agent a in described purificant b to dissolving in, obtaining the cooling bath of the pre-washing agent ab containing obtained dehydrating agent parting liquid c;

To the second separating tank that the purificant b carrying out described cooling is separated with dehydrating agent a;